载钯氧化铝复合材料的制备及性能研究  

Preparation and Property of Palladium/Alumina Composite

作　　者：龙培虹 白天驹 熊良银[2,3] 陈德敏 陈伟[2] LONG Peihong;BAI Tianju;XIONG Liangyin;CHEN Demin;CHEN Wei(School of Materials Science and Engineering,University of Science and Technology of China,Shenyang 110016,China;Shi-Changxu Innovation Center for Advanced Materials,Institute of Metal Research,Chinese Academy of Sciences,Shenyang 110016,China;Key Laboratory of Nuclear Materials and Safety Assessment,Chinese Academy of Sciences,Shenyang 110016,China)

机构地区：[1]中国科学技术大学材料科学与工程学院,辽宁沈阳110016 [2]中国科学院金属研究所师昌绪先进材料创新中心,辽宁沈阳110016 [3]中国科学院核用材料与安全评价重点实验室,辽宁沈阳110016

出　　处：《原子能科学技术》2023年第6期1089-1098,共10页Atomic Energy Science and Technology

基　　金：中国科学院青年创新促进会资助项目;国家自然科学基金(51701226)。

摘　　要：钯常被用作氢同位素分离的首选材料,但纯钯经历多次吸放氢循环后易发生粉化,影响分离系统的效率和工作稳定性,因此实际应用中多采用将钯负载在多孔、疏松载体上的方法抑制钯的粉化。为寻找合适的氢同位素分离材料,本文以多孔氧化铝为载体,采用PdCl_(2)溶液以浸渍还原法制备了钯含量为40.1%(质量分数)的载钯氧化铝复合材料(Pd/Al_(2)O_(3)),并采用X射线衍射(XRD)、BET比表面积、透射电子显微镜(TEM)对其进行了分析,进而对其吸放氢压力组成等温线(PCT)、动力学、热力学及热致吸放氢循环性能进行了测试。结果表明,直径在8~50 nm范围内的钯颗粒存在于氧化铝载体的孔洞内,与纯钯相比,Pd/Al 2O 3复合材料的饱和吸氢量略有降低,吸放氢平台压均升高,平台表现出正斜率,吸氢速率较纯钯提高了5倍,吸放氢焓变和熵变值均降低。经2000次热致吸放氢循环后,Pd/Al 2O 3复合材料的饱和吸氢量和平台压均保持不变,吸氢速率略有提高,未出现钯颗粒的粉化或氧化铝球的破裂,具有良好的抗粉化性能。Palladium is often used as the preferred material for hydrogen isotope separation,but pure palladium tends to be pulverized due to internal stress after repeated hydrogen absorption and desorption cycles.The pulverized palladium particles will increase hydrogen flow resistance,and even block the whole separation system in serious cases,thus affecting the separation efficiency and stability.In order to find suitable materials for hydrogen isotope separation,Pd/Al_(2)O_(3) composite with 40.1%(mass fraction)palladium content was prepared by impregnation-reduction method using porous alumina as carrier and PdCl_(2) solution as palladium precursor.X-ray diffraction(XRD),BET surface area measurement,transmission electron microscope(TEM),and energy dispersive X-ray spectroscopy(EDS)techniques were used to study the phase,specific surface area and pore size distribution,morphology and composition of the material.The kinetics and thermodynamic properties of hydrogen absorption and desorption,hydrogen absorption and desorption cycling properties and anti-pulverization properties were tested by the volumetric absorption/desorption apparatus.Phase analysis results show that the alumina carrier exists in amorphous structure,the supported palladium particles have good crystallinity,and the precursor palladium is fully reduced without introducing other impurities.The results of specific surface area and pore size analysis show that most of the pores in the alumina carrier are mesoporous,the supported palladium exists in the pores of the Al 2O 3 carrier,and the Al 2O 3 carrier can bear a higher amount of palladium.The morphology analysis show that the palladium particles are well dispersed and the size range is from 8 nm to 50 nm.The hydrogen storage performance tests show that compared with the pure palladium,the maximum hydrogen capacity of Pd/Al 2O 3 composites is about 95%of the pure palladium,the plateau pressures of absorption and desorption increase by 21%and 12%separately,and the slope of absorption/desorption plateau i

关 键 词：钯 氧化铝 吸放氢性能 氢同位素分离 

分 类 号：TG139[一般工业技术—材料科学与工程]