Ni系非晶态合金膜的晶化过程与吸氢性能(I)——Ni系非晶态合金膜的DSC、XRD、EXAFS和TPD表征  

Crystallization Process and Hydrogen Adsorption Properties of Ni-Based Amorphous Alloy Membranes(I)——Characterization of DSC, XRD, EXAFS and TPD for Ni-Based Amorphous Alloy Membranes

作　　者：黄森科[1] 刘炳泗[2] 曹勇[3] 邓景发[3] 

机构地区：[1]漳州师范学院化学系,福建漳州363000 [2]辽宁石油化工大学,辽宁抚顺113001 [3]复旦大学,上海200433

出　　处：《石油化工高等学校学报》2003年第3期1-5,共5页Journal of Petrochemical Universities

基　　金：留学回国人员基金;国家自然科学基金资助

摘　　要：　利用改进的化学镀镍技术,制备了对氢具有高选择性和透过性Ni基非晶态合金膜,并用DSC和XRD技术表征了膜的晶化过程。结果表明,Ni-Ru-P非晶态合金膜的热稳定性明显高于Ni-P膜,并且Ni-P合金的晶化过程是由无定形NixPx生成Ni2.55P和Ni的微粒,最后转化为更稳定的Ni和Ni3P结构。EXAFS结果证实,新制备的Ni-P合金膜具有长程无序结构。晶化后,长程无序结构消失。H2-TPD分析发现,Ni-P非晶态合金膜的吸氢性能完全不同于晶化后的Ni-P合金膜。晶化后,Ni-P非晶态合金膜中的粒子聚集和弱的吸附位消失。Ni-based amorphous alloy membranes with higher selectivity and permeability for hydrogen were prepared by an improved electroless Ni-plating. The crystallization processes of the membranes were investigated by means of techniques such as DSC and XRD. The thermal stability of Ni-Ru-P amorphous alloy membranes is obviously higher than that of Ni-P membrane, and the crystallization of Ni-P alloy membrane is completed by two steps, from as-prepared Ni and NixPx to Ni2.55P, then to more stable Ni3P. Meanwhile, EXAFS results prove the existence of a long-range disorder structure in the as-prepared Ni-P amorphous alloy membranes but no such a structure is detected in the Ni-P alloy after crystallization. H2-TPD results indicate that H2 adsorption properties of Ni-P amorphous alloy membrane is completely different from those of Ni-P alloy membranes after crystallization, suggesting that after crystallization the particles aggregate in Ni-P amorphous alloy and the weak adsorption sites disappear on the surface of Ni-P membranes. 

关 键 词：Ni系非晶态合金膜 晶化过程 吸氢性能 DSC XRD EXAFS TPD 表征 电子结构 化学镀镍 

分 类 号：TQ153.12[化学工程—电化学工业]