One-step formation of ZrON thin film on surface of carbon fine particles for membrane electrode assembly

Yudai Aihara, Takashi Iida, Kakeru Kodama, Hiroshi Iwata, Takao Sekiya
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Abstract

Zirconium nitride and oxynitride films were deposited on alumina or carbon particles by reactive sputtering using a magnetron sputtering apparatus with a Zr hollow cylindrical target and a vibrating equipment with heating capability. The vibrating equipment developed in this study was effective if the particles are spherical and highly monodisperse. Uniform film deposition was achieved over the entire surface of highly monodisperse spherical alumina particles using the vibrating equipment during deposition. Pure ZrN crystalline layers was deposited under Ar and N2 gas flows with heating on XC-72 carbon powder particles removed adsorbed oxygen. Energy dispersive x-ray spectroscopy mapping analysis for deposited XC-72 carbon particles showed ubiquitous film deposition on agglomerated particles regardless of vibration during sputtering. Uniform film deposition with vibrating equipment was achieved on the entire surface of CGB-10 particles with more spherical and monodisperse than XC-72 but precipitated crystalline phase depended on unintentional oxygen chemisorbed on the particles. Addition and increase in flow rate of oxygen to the sputtering gas resulted in the formation of desired crystalline phase, Zr2ON2, Zr7O8N4, and monoclinic ZrO2, precipitated in the film using CGB-10 particles with chemisorbed oxygen removed. Current density for oxygen reduction reaction measured for MEA made from CGB-10 particles with ZrON-based crystals deposited was larger than that for thin film deposited on a carbon plate substrate.
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在碳微粒表面一步形成用于膜电极组装的 ZrON 薄膜
使用带有 Zr 中空圆柱靶和具有加热功能的振动设备的磁控溅射装置,通过反应溅射法在氧化铝或碳颗粒上沉积氮化锆和氮氧化物薄膜。如果颗粒是球形且高度单分散,本研究中开发的振动设备就会很有效。在沉积过程中,使用振动设备在高度单分散球形氧化铝颗粒的整个表面实现了均匀的薄膜沉积。纯 ZrN 结晶层是在 Ar 和 N2 气流下沉积的,并在 XC-72 碳粉颗粒上加热除去了吸附的氧气。对沉积的 XC-72 碳颗粒进行的能量色散 X 射线光谱图分析表明,无论溅射过程中振动与否,薄膜沉积在团聚的颗粒上。使用振动设备在 CGB-10 颗粒的整个表面实现了均匀的薄膜沉积,与 XC-72 相比,CGB-10 颗粒更加球形和单分散,但析出的结晶相取决于颗粒上无意化学吸附的氧气。在溅射气体中加入氧气并提高氧气流速,可在使用去除化学吸附氧的 CGB-10 颗粒的薄膜中形成所需的结晶相 Zr2ON2、Zr7O8N4 和单斜 ZrO2。用沉积了 ZrON 基晶体的 CGB-10 颗粒制成的 MEA 所测得的氧还原反应电流密度大于在碳板基底上沉积的薄膜。
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