Hydrogen Permeation Behavior of Zirconium Nitride Film on Zirconium Hydride

Hydrogen permeation barrier plays an important role in reducing hydrogen loss from zirconium hydride matrix when used as neutron moderator. Here, a composite nitride film was prepared on zirconium hydride by in situ reaction method in nitrogen atmosphere. The phase structure, morphology, element distribution, and valence states of the composite film were investigated by XRD, SEM, AES, and XPS analysis. It was found that the composite nitride film was continuous and dense with about 1.6 μm thickness; the major phase of the film was ZrN, with coexistence of ZrO2, ZrO, and ZrN0.36H0.8; and Zr-C, Zr-O, Zr-N, O-H, and N-H bonds were detected in the film. The existence of ZrN0.36H0.8 phase and the bonds of O-H and N-H revealed that the nitrogen and oxygen in the film could capture hydrogen from the zirconium hydride matrix. The hydrogen permeation performance of nitride film was compared with oxide film by permeation reduction factor (PRF), vacuum thermal dehydrogenation (VTD), and hydrogen permeation rate (HPR) methods, and the results showed that the hydrogen permeation barrier effects of nitride film were better than that of oxide film. The zirconium nitride film would be a potential candidate for hydrogen permeation barrier on the surface of zirconium hydride.

High-temperature nitridization of zirconium, production of ceramic and metal-ceramic refractory structures

Based on the results of the work performed, the nature of the phase distribution in the resulting material, structural and morphological differences between the layered metal-ceramic and ceramic structures were established. The temperature range of zirconium nitride synthesis from 1500 to 2400° C is investigated, and the possibility of successful synthesis of nitride ceramics by the indicated method at temperatures significantly exceeding the melting point of the metal is shown.

Effect of Zr content on the structure and morphology of CrZrN thin films prepared by reactive DC magnetron co-sputtering method

In this research, nanostructured chromium zirconium nitride (CrZrN) thin film has been deposited on Si(100) substrates by reactive DC magnetron co-sputtering method without in situ substrate heating and post-deposition annealing. The effects of Zr content on thin film structure and morphology were investigated. The Zr content in the films were varied by applied the sputtering current of Zr target (Izr) in the range of 300 to 900 mA, whereas the current of Cr target was kept at 300 mA. The crystal structure, microstructure, morphology, thickness, and chemical composition were characterized by glancing angle X-ray diffraction (GA-XRD), field emission scanning electron microscopy (FE-SEM), and energy-dispersive X-ray spectroscopy (EDS) techniques, respectively. The results showed that the increase of Izr not only increased the deposition rate, but also increased the Zr content of the as-deposited film ranging from 3.9 to 26.5 at%. The as-deposited thin films were formed as a (Cr,Zr)N solid solution, with fcc structure in (111) and (200) plane, where Cr atoms were replaced by Zr atoms in the CrN lattice. The 2θ diffraction peaks were shifted to the lower value as increase of Zr content which was obtained by increased Izr. The nanocrystalline CrZrN structure with crystal sizes smaller than 10 nm structure were calculated for as-deposited thin films. The lattice parameters increased from 4.187 to 4.381 Å, whereas the crystal size decreased from 8.3 to 6.4 nm. The FE-SEM images of all the CrZrN films exhibited compact columnar with dense morphology as a function of Zr content. Moreover, the thickness of the CrZrN thin films was increased of 302 – 421 nm.

Flash Sintering of Commercial Zirconium Nitride Powders

Flash sintering is an electrical field-assisted densification technique that requires passing a current through a ceramic powder compact. Pressure-assisted flash sintering of commercially available Zirconium Nitride (ZrN) powders has been demonstrated. Near fully dense samples can be obtained within a short period of time. The influences of parameters such as electrical field strength, voltage ramping rate, current limit, external pressure, pre-heating, and holding time on the onset of the flash event were investigated. Some post-flash sintered samples were subjected to the same condition to observe if the material would experience repeated flash. In addition, material properties such as density and hardness were measured and correlated with SEM and XRD. Implications of the observations on underlying flash sintering mechanism will also be discussed.