Abstract The present work describes the economical two-stages catalytic CVD method of the nanocomposite of phosphorous-doped multi-walled carbon nanotubes with nickel (Ni/P-MWCNTs) from the solution of the triphenylphosphine in ethanol using Ni/CaO catalyst. The structure of Ni/P-MWCNTs nanocomposite was studied by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), infrared spectroscopy (IR), X-ray diffraction (XRD), and nitrogen adsorption-desorption method. The Ni/P-MWCNTs nanocomposite are characterized as a mixture of the cylindrical and bamboo-like predominately closed nanotubes with an average outer diameter of 31 nm and SBET=186 m2/g. The P atoms covalently bonded to the carbon framework of the P-MWCNTs walls predominantly through the oxygen bridges. The metal was found in Ni(0) form on the P-MWCNTs tips that is only partially covered by graphene layers. The clusters of bulk Ni(NiO) was also detected in the sample. The glassy carbon electrode modified by the Ni/P-MWCNTs nanocomposite exhibit good electrocatalytic activity in the hexachlorobenzene stepwise degradation and showed an average potential shift of ∼200 mV and ∼130 mV for each stage to the less negative potentials compared to the unmodified glassy carbon electrode and glassy carbon electrode coated by undoped MWCNTs.

中文翻译：

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Ni/P-MWCNTs纳米复合材料的简单两阶段合成作为六氯苯电化学脱氯的有效催化剂

摘要 本工作描述了使用 Ni/CaO 催化剂从三苯基膦的乙醇溶液中制备磷掺杂多壁碳纳米管与镍 (Ni/P-MWCNTs) 纳米复合材料的经济的两阶段催化 CVD 方法。通过高分辨透射电子显微镜（HRTEM）、扫描电子显微镜（SEM）、X射线光电子能谱（XPS）、红外光谱（IR）、X射线衍射（XRD）研究了Ni/P-MWCNTs纳米复合材料的结构，和氮气吸附-解吸法。Ni/P-MWCNTs 纳米复合材料的特征是圆柱形和竹状主要封闭纳米管的混合物，平均外径为 31 nm，SBET=186 m2/g。P 原子主要通过氧桥与 P-MWCNTs 壁的碳骨架共价键合。在 P-MWCNTs 尖端上发现了以 Ni(0) 形式存在的金属，该金属仅部分被石墨烯层覆盖。在样品中也检测到块状 Ni(NiO) 的簇。Ni/P-MWCNTs纳米复合材料改性的玻碳电极在六氯苯逐步降解中表现出良好的电催化活性，与未改性的玻碳相比，每个阶段的平均电位变化为~200 mV和~130 mV至较小的负电位。电极和涂有未掺杂 MWCNT 的玻碳电极。