插层还原法制备纳米钯/石墨烯复合材料的研究

Preparation of Graphene/Pd Nanosized Particle Composites by an Intercalation Reduction Method

摘要:

以氧化石墨和氯化双乙二胺钯Pd(en)2Cl2 为前驱体，将金属钯前驱体与氧化石墨发生插层反应，再将插层了Pd(en)22+的氧化石墨在溶液中用NaBH4还原，制备出纳米钯/石墨烯复合材料。采用X射线衍射(XRD)、场扫描电子显微镜(FE-SEM)、透射电子显微镜(TEM)、电感耦合等离子体发射光谱(ICP)、低温氮气吸附等手段对复合材料进行表征并对复合材料进行了储氢性能的测试。研究结果表明：复合材料具有规则的中孔结构，直径为2~6 nm钯的纳米粒子弥散地分布在石墨烯的层间，起着支撑作用，阻止石墨烯片层的重新聚集；复合材料具有较高的BET比表面积，在77 K及0.11 MPa条件下其储氢量达到了3.4%（质量分数）。

Abstract:

Using Pd(en)2Cl2 as the Pd precursor and graphite oxide as the carbon precursor, the Pd(en)22+ intercalated graphite oxide was synthesized, then it was reduced in solution with NaBH4 and the graphene/Pd nanosized particle composites were obtained. The final graphene composites were characterized by XRD, FE-SEM, TEM, ICP and N2 adsorption test and their H2 storage property was also measured. The results show that the composites have a regular mesoporous structure, and Pd particles with a diameter of 2~6 nm are evenly dispersed between graphene sheets and pillar the graphene sheets to inhibit the accumulation of grapheme sheets. The composites have a high BET surface area and their H2 storage reaches 3.4 wt% at 77 K and 0.11 MPa.