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Pd-Cu合金复合膜的制备及表征

Preparation and Characterization of Pd-Cu Alloy Composite Membranes

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【作者】 高会元李永丹林跃生

【Author】 GAO Hui-yuan~(1,2),LI Yong-dan~1,LIN Yue-sheng~(1,3) (1 Department of Catalysis Science and Engineering,School of Chemical Engineering,University of Tianjin,Tianjin 300037,China;2 Department of Applied Chemistry,School of Chemical Engineering and Biological Technology,Hebei Polytechnic University,Tangshan 063009,Hebei,China;3 Department of Chemical and Materials Engineering,Arizona State University,Arizona AZ 85287-1066,USA)

【机构】 天津大学化工学院催化科学与工程系天津大学化工学院催化科学与工程系 天津300037河北理工大学化工与生物技术学院应用化学系河北唐山063009天津300037美国亚利桑那大学化工与材料工程系亚利桑那州AZ85287-1066

【摘要】 采用无电化学镀技术制备了Pd-Cu合金复合薄膜。复合膜的初始基体是0.2μm等级的316L多孔不锈钢圆片(PSS),经过改性的(含Pd)溶胶-凝胶ZrO2成膜技术对PSS表面进行了修饰。修饰后的PSS表面首先进行无电镀金属Pd膜,然后在Pd膜表面再镀金属Cu膜。最后把具有双金属镀层的膜片在773 K,H2气氛(101kPa)下保持5~10h进行退火热处理,通过金属间分子热扩散把不锈钢基体上的金属Pd膜和金属Cu膜合金化为均匀的Pd-Cu合金复合薄膜。XPS确定表面组成为Pd90Cu10(质量分数/%)合金薄膜,经过XRD分析结合确定为单相无序fcc结构;而Pd59Cu41合金膜是由平衡fcc相和有序bcc相组成。通过SEM观察到Pd90Cu10合金薄膜(厚度5μm)表面存在一些针孔;而Pd59Cu41合金膜(厚度10μm)没有针孔存在,这种合金复合膜应该具有极高的透H2选择性。

【Abstract】 Thin Pd-Cu/ZrO2-PSS composite membranes were prepared by modified electroless plating technique on 0.2 μm graded 316L porous stainless steel(PSS) disks.After the surface of PSS was modified by Pd-doped zirconia,the zirconia side of the modified support was successively coated with palladium and copper by electroless plating.Finally,the as-deposited Pd-Cu/ZrO2-PSS composite membrane was annealed in hydrogen at 773K for 5~10h in order to form a homogeneous palladium-copper alloy film by thermal diffusion.XPS analyses showed the average surface composition of the two membranes were respectively Pd90Cu10 and Pd59Cu41(mass fraction/%).XRD analyses indicated that deposited Pd90Cu10 alloy film contained only fcc(face-centred cubic) phase structure whereas Pd59Cu41 alloy film contained a mixture of fcc and bcc(body-centred cubic phase).Surface micrographs made by SEM showed the presence of some visible pin-holes on the 5μm thick Pd-Cu/ZrO2-PSS membrane, and pinhole free surface for the 10μm one which should possess an excellent perm-selectivity for hydrogen.

【基金】 长江学者奖励计划项目(411015);海外杰出青年基金项目(50228203)
  • 【文献出处】 材料工程 ,Journal of Materials Engineering , 编辑部邮箱 ,2006年02期
  • 【分类号】TB383.2
  • 【被引频次】12
  • 【下载频次】312
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