Microstructure of polyfuran/perchlorate-doped films by scanning and transmission electron microscopies and electron diffraction

Microstructure of polyfuran/perchlorate-doped films by scanning and transmission electron microscopies and electron diffraction
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DOI:
10.1021/ma960101a
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发表时间:
1996
期刊:
影响因子:
5.5
通讯作者:
I. Carrillo;C. Barba;M. J. González-Tejera;I. Hernández-Fuentes
I. Carrillo;C. Barba;M. J. González-Tejera;I. Hernández-Fuentes
中科院分区:
化学1区
文献类型:
--
作者:
I. Carrillo;C. Barba;M. J. González-Tejera;I. Hernández-Fuentes

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采用扫描电镜、透射电镜和电子衍射技术对高氯酸根掺杂的聚呋喃薄膜(PFu/ClO 4)进行了形貌和微结构分析。在乙腈/高氯酸钠介质中,在铂电极上,在恒电位下进行电化学成膜,E d = 2.6 V(Ag/Ag +)。薄膜表面形貌的研究表明,薄膜生长面为有序的球状结构,球状结构的大小取决于Ed。结节的排列遵循平行于衬底的方向。透射电镜和选区微电子衍射结果表明,在PFu/ClO 4薄膜的横截面和平面截面上,均发现了结晶结构嵌入非晶畴中。靠近薄膜生长表面的平面部分表现出随机取向的晶体,而在更深的层中检测到具有层状结构的单晶。在平面和横截面中获得的电子衍射图案与六方晶胞一致:α = 0.68 nm和c = 0.62 nm,α = β = 90°和γ = 120°。在平面截面上存在的莫尔条纹证实了PFu/ClO 4薄膜的层状结构。
Polyfuran films doped with perchlorate anions (PFu/ClO 4 ) were studied by scanning and transmission electron microscopies and electron diffraction in order to analyze their morphology and microstructure. Film generation was carried out electrochemically at constant potential, E d = 2.6 V (Ag/Ag + ), onto platinum electrodes in acetonitrile/sodium perchlorate medium. The study of the superficial films morphology revealed an ordered nodular structure in the films growth face, the nodular size depending on E d . Alignment of nodules followed a direction parallel to the substrate. Crystalline structures immersed in amorphous domains were found in planar sections and cross-sections of PFu/ClO 4 films by transmission electron microscopy and selected area micro-electron diffraction. Planar sections close to the film growth surface exhibited randomly oriented crystals, while single crystals with lamellar structures were detected in deeper layers. Electron diffraction patterns obtained in planar and transversal sections were consistent with a hexagonal unit cell : α = 0.68 nm and c = 0.62 nm, α = β = 90°, and γ = 120°. The existence of moire patterns in planar sections confirms the laminar structure proposed for PFu/ClO 4 films.