Abstract

A simple process to synthesize metal nitride particles was proposed using submerged arc discharge plasma in liquid nitrogen. Gibbs standard free energy was considered for the selection of the nitride-forming materials. In this study, titanium (Ti) and aluminum (Al) electrodes were used as raw materials for nitride particle preparation. Liquid nitrogen acted as a dielectric medium as well as a nitridation source in this process. A copper electrode was also used as a non-reactive material for comparison with the reactive Ti and Al electrodes. As the operating conditions of the experiments, the arc discharge current was varied from 5 A (low-power mode) to 30 A (high-power mode). The formation of titanium nitride (TiN) and aluminum nitride (AlN) was confirmed in the particles prepared in all experimental conditions by X-ray powder diffraction (XRD). The observation using a field emission scanning electron microscope (FE-SEM) and a field emission transmission electron microscope (FE-TEM) indicated that the synthesized TiN particles showed a cubic morphology, whereas AlN particles containing unreacted Al showed a spherical morphology. The experiments using different metal electrode configurations showed that the anode generated most of the particles in this process. Based on the obtained results, a particle formation mechanism was proposed.

Highlights

  • Of the synthesized nanoparticles observed by a field operation with SU9000, The the morphologies samples of Al were coated with osmiumwere (Os) with approxiemission transmission electron microscope (FE-TEM, JEM-2010F, Jeol mately 5 nm thickness using Os plasma coating (Neoc-pro, Meiwafosis, Tokyo, Japan) The crystalline particles were identified by a selected-area electron diffraction (SAED) pattern

  • The results indicated that the crystallinity of synthesized titanium nitride (TiN) was enhanced with increasing the current

  • The X-ray powder diffraction (XRD) patterns showed that when the current increased, the intensities of aluminum nitride (AlN) peaks increased, while those of Al peaks decreased, 13 of 23 current, indicating that the crystallinity of synthesized AlN was enhanced with increasing similar to the Ti experiments

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Summary

Introduction

Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affiliations. Investigated the effect of discharge behavior by changing the electrode material As a product, they obtained Al, Ti, V, Fe, Ni, Cu, Zr, Nb, Mo, Ta, and W micro-size particles using a DC power supply [36]. Some studies have been reported to synthesize carbon-based functional materials [44] Most of these studies focused on plasma behaviors and their effects on the electrodes and products. As a novel and simple process for metal nitride particle preparation, submerged arc discharge plasma in liquid nitrogen was used, where liquid nitrogen acted as a nitrogen source as well as a dielectric medium. Nitride fine particles were synthesized from the electrode directly by submerged arc discharge in liquid nitrogen.

Selection of Metal Electrodes
Preparation of Metal Nitride Particles
Detailed operating
Characterization
Figure shows the theparticles
Results
FE-TEM Observation
30 A and corresponding
TEM images images of Ti
Crystallite Phase of the Synthesized TiN Particles
Crystallite
In the determination of
Crystallite Phase of the Prepared Cu Particles
Morphologies of the Prepared Particles
Crystallite Phase of the Synthesized Particles
16. X-ray patterns of theof
Mechanism of Formation
Findings
Thermion Emission from the Cathode
Conclusions
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