Cl-assisted highly efficient synthesis of FePd3 alloys encapsulated in graphite papers: a two stage CVD approach

Cl-assisted highly efficient synthesis of FePd3 alloys encapsulated in graphite papers: a two stage CVD approach
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Cl 辅助高效合成石墨纸封装的 FePd3 合金:两阶段 CVD 方法

DOI:
10.1039/c6ra04777g
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发表时间:
2016-04
期刊:
影响因子:
3.9
通讯作者:
Filippo S· Boi
Filippo S· Boi
中科院分区:
化学3区
文献类型:
--
作者:
Filippo S· Boi

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最近的研究表明,通过在二茂铁中添加二氯环辛二烯钯,可以将FEPD合金包覆在石墨碳基体系中,以获得更好的粒子分散性。在这里,我们提出了一种先进的两步法,它允许在整个反应堆中合成以FePd3合金填充的非常厚的平面卷曲状石墨结构的沉积。第一阶段用于在Si/SiO_2衬底上热解含Pd的碳氢化合物以沉积Pd,第二阶段用于蒸发和热解FEPD合金形成和包覆的含铁前驱体(二茂铁)。退火研究还表明,在Ar/H2气流中,在600-650°C条件下,即使经过数十小时,FePd3结构的晶胞也没有变化。相反,发现包裹的颗粒形状和空间排列发生了变化。通过扫描和透射电子显微镜、能量色散X射线、拉曼光谱、热重分析、X射线衍射仪和室温磁强计对样品进行了详细的表征。
Recently it has been shown that FePd alloys can be encapsulated in graphitic carbon based systems for a better particle dispersion through addition of dichloro-cyclooctadiene palladium to ferrocene. Here we propose an advanced two-stage method which allows the synthesis of very thick deposits of planar rolled-like graphite structures filled with FePd3 alloys as dominant product in the entire reactor. The first stage is used to pyrolyze the Pd-containing hydrocarbon on the top of Si/SiO2 substrates for Pd deposition while the second stage is used for the evaporation and pyrolysis of the Fe-containing precursor (ferrocene) for the FePd alloy formation and encapsulation. Annealing studies also show that no changes in the unit cell of the FePd3 structure are found even after tens of hours at 600–650 °C under Ar/H2 flow. Instead a change in the encapsulated particle shape and spatial arrangement is found. The samples are characterized in detail through scanning and transmission electron microscopy, energy dispersive X-rays, Raman spectroscopy, thermogravimetric analyses, X-ray diffraction and room-temperature magnetometry.
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