Fabrication and characterization of highly ordered porous alumina
templates by a two-step anodization process.
C. A. León-Patiño
a
, E. A. Aguilar-Reyes
b
, C. Ruiz-Aguilar
c
Instituto de Investigaciones Metalúrgicas, Universidad Michoacana de San Nicolás de Hidalgo
Ed. “U”, Ciudad Universitaria, Morelia Mich., Mexico
a
caleon@umich.mx,
b
aareyes@umich.mx,
c
ziru_3@hotmail.com
Keywords: anodic alumina, porous templates, anodization, nanopore, auto-ordered structure
Abstract. Highly ordered through-hole anodic porous alumina membranes were fabricated by
electrochemical oxidation of aluminum in a controlled two-step process. A teflon dispositive was
used to ensure single side anodization. Under the most appropriate condition for the fabrication of
ideally ordered anodic aluminum oxide (AAO), the voltage used was 15 V during 24 h in a 15 %
w/v sulfuric acid solution. SEM, TEM and FESEM characterization shows that the as-fabricated
AAO film has a defect-free array of straight parallel channels perpendicular to the surface. The
thickness of the porous membrane is 20 microns, approximately. The ordered channels are formed
in a honey comb arrange with a pore diameter in the range 20-30 nm, wall thickness of 10-20 nm,
interpore distance of ∼40 nm, and high aspect ratio of 850. The pore density, quantified by image
analysis, is 5.4×10
10
pore/cm
2
; perfect ordering was maintained in the full depth of the membrane.
Dimensions of this porous structure provide a convenient way to precision engineer the nanoscale
morphology.
Introduction
Anodic aluminum oxide (AAO) is a self-organized nanostructured material containing a high
density of uniform cylindrical pores that are aligned perpendicular to the surface of the materials
and penetrate its entire thickness. In recent years, electrochemical processes have been widely used
to fabricate materials with nanostructured arrangements. Their miniaturizing capacity and attractive
structure made them suitable for new areas of applications in the fields of nanofilters [1], magnetic
storage [2], solar cells [3], metal and carbon nanowires [4], and catalysis [5]. Given the uniformity
of the porous channels and capacity to tailor their aspect ratio, the AAO templates with high pore
densities are more versatile and economical than those obtained by sophisticated methods as
lithography. The porous alumina nanostructures obtained by electrochemical oxidation of aluminum
are sensible to experimental parameters as temperature, voltage, type and concentration of the
electrolyte, and anodization time [6]. Since during the anodization process the aluminum film is
immersed and exposed in its entire surface to the electrolyte solution, the dense aluminum oxide
that results of the electrochemical reaction is trapped in the middle part of the membrane when the
porous structures grow in opposite directions in both sides of the membrane [6-8]. This mechanism
prevents to obtain open and continuous pores along the thickness of the membranes. The present
work propose the synthesis of highly ordered through-hole anodic porous alumina membranes by a
two-step anodization process of aluminum in sulfuric acid using a teflon dispositive specially
designed to ensure single side anodization. The structure parameters of the resulting porous AAO
membranes are studied by image analysis using different microscopy techniques.
Experimental Procedure
Synthesis of the auto-ordered AAO membranes. The porous AAO membranes were synthesized
by a two-step aluminum anodization process. It started from ultra-high purity aluminum films (Alfa
Aldrich, 99.9%, 100 µm thickness), which were sectioned in specimens of 1.5×1.5 cm for the
anodes; the anodized area was 1×1 cm. As the cathode, it was used 6061 commercial aluminum
film. Both electrodes were welded to aluminum extension wires of 1/32 inch to be connected to a
Materials Science Forum Vol. 755 (2013) pp 75-81
Online available since 2013/Apr/24 at www.scientific.net
© (2013) Trans Tech Publications, Switzerland
doi:10.4028/www.scientific.net/MSF.755.75
All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP,
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