The application of ultramicrotomy to the electronoptical examination of surface films on aluminium

Furneaux, R. C.; Thompson, G.E.; Wood, G. C.

doi:10.1016/0010-938x(78)90009-4

Cited by 239 publications

(50 citation statements)

References 15 publications

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“…For ultramicrotomy, the specimens were trimmed initially with a glass knife and final sections were generated with a diamond knife. [12] 235 Enrichment, incorporation and oxidation of copper during anodising As expected, [6,7] increasing LP generated an oxide with finer pores in the external regions of the anodic oxide film, generated during the early stages at low potentials, and larger pores in the internal regions, generated later at increased potentials. Accordingly, decreasing LP resulted in larger pores in the external regions (generated at high potentials) and finer pores in the internal regions (generated later at reduced potentials).…”

Section: Methodsmentioning

confidence: 75%

Enrichment, incorporation and oxidation of copper during anodising of aluminium–copper alloys

Curioni

Roeth

Garcia-Vergara

et al. 2009

Surface & Interface Analysis

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Porous anodic oxides generated on copper-containing aluminium alloys are less regular than anodic oxides generated on pure aluminium. Specifically, a porous oxide morphology comprising layers of embryo pores, generated by a cyclic process of oxide film growth and oxygen evolution, is generally observed. In this work, the relation between the oxidation behaviour of copper during anodising and the specific porous oxide film morphology was investigated by electrochemical techniques, transmission electron microscopy and Rutherford backscattering spectroscopy (RBS). It was found that the anodising potential determines the oxidation behaviour of copper, and the latter determines the porous oxide morphology. At low voltage, relatively straight pores with continuous cell walls were obtained on Al-Cu alloys, but selective oxidation of aluminium atoms resulted in the occlusion of copper-containing metallic nanoparticles in the anodic film. At higher potentials, copper oxidation promoted oxygen evolution within the barrier layer, and generation of a less regular film morphology. RBS, performed on Al-Cu alloy specimens, revealed a high volume fraction of copper atoms in the anodic films generated at low potentials and a reduced amount of copper atoms in the anodic oxide films generated at high potentials.

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Section: Methodsmentioning

confidence: 75%

Enrichment, incorporation and oxidation of copper during anodising of aluminium–copper alloys

Curioni

Roeth

Garcia-Vergara

et al. 2009

Surface & Interface Analysis

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“…Barrier anodic oxide films and porous anodic oxide films on aluminum have been widely investigated by many researchers in the fields of surface finishing [1][2][3], electrolytic capacitor application [4][5][6], and micro-and nano-structure fabrication [7][8][9]. Recently, highly ordered anodic porous alumina with a cell size on the scale of 10-100 nm has been studied for potential use in various ordered-nanostructure applications [10][11][12][13][14][15][16][17][18][19][20][21].…”

Section: Introductionmentioning

confidence: 99%

Self-Ordering Behavior of Anodic Porous Alumina via Selenic Acid Anodizing

Kikuchi

Nishinaga

Natsui

et al. 2014

Electrochimica Acta

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The self-ordering behavior of anodic porous alumina that was formed by anodizing in selenic acid electrolyte (H 2 SeO 4 ) at various concentrations and voltages was investigated with SEM and AFM imaging. A high purity aluminum foil was anodized in 0.1-3.0 M selenic acid solutions at 273 K and at constant cell voltages in the range of 37 to 51 V. The regularity of the cell arrangement increased with increasing anodizing voltage and selenic acid concentration under conditions of steady oxide growth without burning. Anodizing at 42-46 V in 3.0 M selenic acid produced highly ordered porous alumina. By selective dissolution of the anodic porous alumina, highly ordered convex nanostructures of aluminum with diameters of 20 nm and heights of 40 nm were exposed at the apexes of each hexagonal dimple array. Highly ordered anodic porous alumina with a cell size of 102 nm from top to bottom can be fabricated by a two-step selenic acid anodizing process, that includes the first anodizing step, the selective oxide dissolution, and the second anodizing step.Key words: Aluminum; Anodizing; Anodic Porous Alumina; Selenic Acid IntroductionBarrier anodic oxide films and porous anodic oxide films on aluminum have been widely investigated by many researchers in the fields of surface finishing [1][2][3], electrolytic capacitor application [4][5][6], and micro-and nano-structure fabrication [7][8][9]. Recently, highly ordered anodic porous alumina with a cell size on the scale of 10-100 nm has been studied for potential use in various ordered-nanostructure applications [10][11][12][13][14][15][16][17][18][19][20][21]. Anodic porous alumina is typically fabricated on an aluminum substrate using electrochemical anodizing (or anodization) [22][23][24][25][26]. In several acidic electrolyte solutions, the porous alumina fabricated by anodizing is self-ordered when prepared at the appropriate electrochemical conditions, including appropriate concentrations, temperatures, and voltages (or electrochemical potentials) [27][28][29][30] [50], and acetylenedicarboxylic (HOOC-C≡C-COOH) [51] acids have also been reported as electrolytes used to fabricate porous alumina that has characteristic nanostructure morphologies.In addition to these acidic electrolytes, alkaline and neutral solutions used for porous alumina fabrication were reported by several research groups. Takahashi et al. reported that a porous anodic oxide film could be formed by anodizing in an H 3 BO 3 /Na 2 B 4 O 7 neutral borate solution at a high temperature [52]. Baron-Wiechec et al. investigated aluminum anodizing in a borax (Na 2 B 4 O 7 ) solution at 333 K and successfully obtained porous alumina [53]. Noguchi et al. investigated the anodizing behavior of aluminum in propylenediamine and choline alkaline solutions containing ammonium fluoride, ammonium tartrate, ammonium carbonate, and ammonium tetraborate, and obtained anodic porous alumina with nanopores that were 10-150 nm in diameter [54]. However, it is difficult to form a highly ordered porous alumina by anodiz...

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“…The sections were prepared by ultramicrotomy, 17 with nominal thickness of 10 nm. The compositions of specimens were determined by Rutherford backscattering spectroscopy (RBS), using 1.9 or 2.0 MeV He C ions from the Van de Graaff accelerator of the University of Paris.…”

Section: Methodsmentioning

confidence: 99%

A tracer investigation of chromic acid anodizing of aluminium

Garcia-Vergara

Skeldon

Thompson

et al. 2007

Surface & Interface Analysis

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A tungsten tracer introduced into a sputtering-deposited aluminium substrate was employed to investigate pore development in anodic films formed at 3 mA cm −2 in 0.25 M chromic acid electrolyte at 313 K. The anodized specimens were observed by transmission electron microscopy (TEM), with compositions of films determined by Rutherford backscattering spectroscopy (RBS). The anodic films were found to be similar in thickness to that of the aluminium layer consumed during anodizing and revealed the feathered pore morphology that is a characteristic of the electrolyte. The anodizing efficiency was ∼45-48%, with tungsten tracer species, in addition to aluminium species, being lost to the electrolyte at the pore base. These findings, together with the relatively uniform distribution of tungsten species within the film, are consistent with field-assisted dissolution of the alumina playing a major role in the development of pores. The films contrast with those formed in phosphoric and sulphuric acid electrolytes, for which feathering of pores is absent, the tracer distribution is inverted and the film thickness exceeds that of the consumed metal, features indicative of the influence of material flow in pore development.

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The application of ultramicrotomy to the electronoptical examination of surface films on aluminium

Cited by 239 publications

References 15 publications

Enrichment, incorporation and oxidation of copper during anodising of aluminium–copper alloys

Enrichment, incorporation and oxidation of copper during anodising of aluminium–copper alloys

Self-Ordering Behavior of Anodic Porous Alumina via Selenic Acid Anodizing

A tracer investigation of chromic acid anodizing of aluminium

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