脱合金法制备纳米多孔铜的研究

发布时间：2018-07-10 15:18

本文选题：纳米多孔铜 + 薄膜　；参考：《济南大学》2011年硕士论文

【摘要】：冶金学认为脱合金是在腐蚀环境中选择性地除去合金中较活泼组元的一种腐蚀现象。但是它也可以被用来制备具有三维结构材料、薄膜材料和一维纳米线等低密度的纳米多孔金属材料。纳米多孔金属开拓了金属材料新的应用,将材料的多孔形态与物理、化学、机械性能结合起来,超越材料固有功能,发挥多孔材料的轻质、高强韧、强吸附、隔热、散热、优异的吸能性能等一系列特性,具有结构和功能双重作用,被广泛用于催化、化学、生物传感、燃料电池电极、汽车、海洋采油、航空航天等领域。因此材料的微观结构设计,对多孔金属材料的工程应用和设计开发具有深远的影响意义。本论文采用两种方法制备了前躯体母合金,一是磁控溅射法,二是单辊旋淬法。研究内容和结论如下: (1)使用磁控溅射法在玻璃和单晶硅两种不同的基底上沉积铜锌合金薄膜。通过改变三个工艺参数--溅射电流、溅射压强以及溅射时间,来研究这些参数对薄膜的组元分布、厚度、表面形貌、表面粗糙度、电阻率变化及稳定性的影响,获得最佳工艺参数。 (2)以Cu62Zn38合金薄膜为前躯体母合金,在H_2SO_4溶液中脱合金化处理后制备多孔纯铜薄膜,采用X射线衍射分析、扫描电镜、EDS能谱分析等手段研究合金的结构及以其为母合金的脱合金化后所得多孔铜的多孔结构和断口形貌,研究了酸溶液浸泡处理对多孔铜的多孔结构的影响。实验结果表明:磁控溅射沉积薄膜出现非晶特征;在稀H_2SO_4溶液中进行脱合金化腐蚀后,两相中的Zn元素被腐蚀掉,制备出连续纳米多孔结构的铜薄膜材料。Cu62Zn38合金在2 mol/L H_2SO_4溶液和7 mol/L H_2SO_4溶液中是非均匀腐蚀,在2 mol/L H_2SO_4溶液中形成的纳米孔的密度较小,而且有些区域尚未成孔;薄膜在7 mol/L H_2SO_4溶液中腐蚀时,薄膜整体从基底剥落并发生卷曲,表明脱锌层引起的内应力超过表面附着力使薄膜发生断裂且卷曲,层状卷曲的薄膜不能充分腐蚀,难以形成均匀的多孔结构薄膜;在5 mol/L H_2SO_4溶液中为均匀腐蚀,形成铜骨架和孔结构,部分孔呈现蜂窝状,其骨架尺寸51～228nm,平均尺寸约为92.7nm,平均孔径尺寸约为94nm,形成一个内部连续三维的网络状结构。 (3)以Zn10Cu90和Zn20Cu80合金为前躯体母合金,分别在盐酸和硫酸中脱合金处理,制备块状纳米多孔铜,采用X射线衍射分析、扫描电镜、EDS能谱分析等手段研究合金的多孔结构和断口形貌。实验结果表明:Zn10Cu90和Zn20Cu80合金带由主要由Cu0.64Zn0.36(α相)和CuZn电子化合物(β相)两相组成,Cu0.64Zn0.36和CuZn电子化合物被完全除去,形成了大孔结构的纳米多孔结构。块状纳米多孔铜是带系和孔道组成的双连续、开孔结构,高孔隙率使材料具有高强度、低密度的纳米多孔结构。另外,细小的棒状块体和切片也可使用脱合金方法制备出纳米多孔材料。通过对两种制备纳米多孔铜工艺的对比分析,探讨了脱合金法制备多孔材料的机制,对于今后制备和研究纳米多孔材料具有一定的借鉴作用。
[Abstract]:The nano porous metal is used for preparing nano porous metal material with low density , such as three - dimensional structure material , thin film material and one - dimensional nano wire .

In this paper , the precursor master alloy is prepared by two methods , one is magnetron sputtering method , two is single roller spinning quenching method . The research contents and conclusions are as follows :

( 1 ) Using magnetron sputtering method to deposit copper - zinc alloy thin films on two different substrates of glass and monocrystalline silicon . By changing the parameters of three parameters - sputtering current , sputtering pressure and sputtering time , the effects of these parameters on the distribution , thickness , surface morphology , surface roughness , resistivity change and stability of the films are studied .

( 2 ) The porous pure copper thin films were prepared by de - alloying in H _ 2SO _ 4 solution with Cu62Zn38 alloy thin film as precursor master alloy . The results showed that the thin films formed in the solution of 2 mol / L H2SO4 and 7 mol / L H _ 2SO _ 4 were non - uniform . The results showed that the films could not be fully corroded in 2 mol / L H _ 2SO _ 4 solution .

( 3 ) The porous structure and fracture morphology of the alloy were investigated by using Zn10Cu90 and Zn20Cu80 alloys as precursor master alloys . The results show that the Zn10Cu90 and Zn20Cu80 alloy bands are composed of two phases : Cu0.64Zn0 . 36 ( 伪 phase ) and CuZn electronic compound ( 尾 phase ) . The experimental results show that the Cu0.64Zn0 . 36 and CuZn electronic compounds are completely removed to form the nano porous structure with large pore structure .

Through the comparative analysis of the two methods for preparing the nano porous copper , the mechanism of preparing the porous material by the dealloying method is discussed , which can be used for reference for the preparation and research of the nano porous material in the future .
【学位授予单位】：济南大学
【学位级别】：硕士
【学位授予年份】：2011
【分类号】：TB383.1

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