Nanopore formation and growth in phosphoric acid Al anodization (original) (raw)
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ACS applied materials & interfaces, 2015
The pores growth mechanism and their self-ordering conditions are investigated for nanoporous alumina membranes synthesized by Hard Anodization (HA) of Al in a broad range of anodic conditions, covering oxalic acid electrolytes with concentrations from 0.300 M down to 0.075 M, and potentiostatic anodization voltages between 120 and 225 V. The use of Linear Sweep Voltammetry (LSV), scanning and transmission electron microscopy, together with image analysis techniques allow to characterize the intrinsic nature of the HA regime. HA of aluminum is explained on the basis of a phenomenological model taking into account the role of oxalate ions and their limited diffusion through alumina nanochannels from bulk electrolyte. The depletion of oxalate ions at the pores bottom causes an increased growth of the alumina barrier layer at the oxide/electrolyte interface. Furthermore, an innovative method has been developed for the determination of the HA conditions leading to self-ordered pores gro...
Effect of Formation Voltage on the Pore Size of Porous Anodic Aluminum Oxide
IOP Conference Series: Materials Science and Engineering
This work is aimed to clarify the effect of formation voltage on the pore size of porous anodic aluminum oxide (PAAO) layer formed on commercially pure aluminum. The PAAO layers were obtained by anodization process in 0.3 M sulfuric acid solution at constant voltages of 10, 15, 20, and 25 V at 10°C. The structure and morphology of PAAO layers were characterized by using FE-SEM. The pore diameters which were estimated by using ImageJ software were 19.61 + 15.35 nm, 20.03 + 13.59 nm, 20.31 + 12.36 nm, 25.06 + 12.10 nm, and the wall thicknesses were 33 nm, 49.99 nm, 74.97 nm, 83.33 nm for the PAAO formed at 10, 15, 20 and 25V, respectively. The structure of the porous oxide layer became more uniform and organized, and the diameter of the pores increased linearly with applied voltage. High anodization voltage is known to cause Joule heating because of the fast movement of electrons and ions. It is believed that the Joule heat was transferred to the bulk electrolyte which results in larger pore diameter and interpore distance. The optimum condition to obtain high order PAAO is at 25 V.
Formation of nanoscale pore arrays during anodization of aluminum
Europhysics Letters (EPL), 2005
A theory of the spontaneous formation of spatially regular hexagonal arrays of nanopores in aluminum oxide film growing during aluminum anodization is presented. Linear stability analysis shows that, in certain ranges of the applied voltage and electrolyte pH, the oxide film is unstable with respect to perturbations with a well-defined wavelength. The instability is caused by a positive feedback between the oxidation-dissolution rates and variations of electric field caused by perturbations of the metal-oxide and oxide-electrolyte interfaces. The competition between this instability and the stabilizing effects of the Laplace pressure and elastic stress provides the wavelength selection mechanism. The hexagonal ordering of pores results from the resonant quadratic nonlinear interaction of unstable modes.
Materials Letters, 2013
A simple method of fabrication of anodic aluminum oxide at low voltages (from 5 to 15 V) in 0.3 M oxalic acid is presented. To overcome the issues concerning the anode's burning, a high velocity stirring was applied. It allowed to achieve nanopores with ultra-small diameters (even 12 nm), interpore distance (even 31 nm) and tremendously high pore densities (up to 980 pores per 1 mm 2 ) with simultaneous high porosity (up to 38%). Moreover, the presented approach (no modifier added to the electrolyte) resulted in the AAO with relatively well arranged ultra-small nanopores.
The Review of scientific instruments, 2015
A new electrochemical setup and the associated procedures for growing ordered anodic aluminum oxide pore arrays on large surfaces are presented. The typical size of the samples is 14 × 14 cm(2). The most crucial experimental parameters that allow for the stabilization of the high-field procedures are a very efficient cooling of sample and electrolyte, as well as the initial ramping up of the voltage at an accurately defined rate. The morphology of the cylindrical, parallel alumina pores is similar to those obtained on smaller scales with standard setups. Our setup facilitates the availability of porous anodic alumina as a template system for a number of applications.
2015
Department of Chemistry, Maharshi Dayanand University, Rohtak-124 001, Haryana, India E-mail : vermanaveen17@gmail.com Departament de Física Aplicada, Universitat Politècnica de València, 46022 València, Spain Manuscript received online 27 November 2014, revised 05 December 2014, accepted 05 December 2014 Porous anodic alumina (PAA) is a versatile template for the fabrication of nanomaterials. To obtain highly ordered nanopore array, two step anodization process is a much less expensive method than other methods like lithography, optical diffraction grating etc. The PAA template was fabricated by two step anodization process. The first step proceeded in oxalic acid to different extent of anodization time and at different voltages to predict the influence of anodization conditions in the first step on the morphology and microstructure of porous anodic alumina film formed in phosphoric acid in the second step. The time varied from 10 to 120 min and voltage varied from 20 to 50 V in th...
Journal of Materials Science and Engineering B, 2015
The effect of voltage on nanopores formed via electrochemical anodization of high purity Aluminum was investigated. The electrochemical bath consisted of a 0.3 M oxalic acid electrolyte. A platinum electrode was used as the counter-electrode, and an aluminum sheet as the anode. The anodization process was carried out at a temperature of 7 °C at various voltages ranging from 30 to 55V. It was observed that during the anodizing process, both the current density and the nanopore size increase as the applied voltage increases. The morphology and the distribution of nanopores were analyzed by SEM (Scanning electron microscope). It was found that mean pore diameter increased from 43 to 100 nm as the voltage is increased from 30 to 55 V. the polydispersity of the pore size was found to be minimum at 40 V.
Room Temperature Anodization of Aluminum at Low Voltage
2013
Membranes with nanometer-scale features have many applications, such as in optics, electronics, catalysis, selective molecule separation, filtration and purification, biosensing, and single-molecule detection. Anodiztion process was conducted using 15, 20, 30 and 35% by volume phosphoric acid. Results showed that Porous Anodized Aluminum (PAA) with ideal nanopore arrays can be fabricated at room temperature by one-step anodization on high purity aluminum foil at 5V. Morphology of the PAA was characterized by scanning electron microscopy (SEM). The electrochemical behavior of anodized aluminum was studied in 0.1M Na2SO4 solutions using electrochemical impedance spectroscopy (EIS). The highest resistance of the porous layer (Rp) was detected for the samples anodized in 20% phosphoric acid.
Nanopore formation dynamics during aluminum anodization
Physica D: Nonlinear Phenomena, 2007
This paper predicts the evolution of nanopores during anodic oxidation of aluminum. The theory is based on approximate nonlinear evolution equations of the interfaces, which reproduce all the observed patterns, and using them for stability analysis. The pore structure in the early stages is described by the Damped Kuramoto-Sivashinsky (DKS) equation, which predicts hexagonal patterns with points and line defects, in agreement with experimental observations of the evolving pores. This is the first work to follow pore dynamics. Comparison with asymptotic constant-thickness and -curvature solutions is conducted.
Ultrasmall nanopores obtained by electric field enhanced one-step anodisation of aluminium alloy
Surface and Coatings Technology, 2014
The influence of electric fields at different temperatures on the anodic oxide layer growth was studied on AA 5083. Barrier-type alumina layers showed a fair morphology with multiform pores. The diameter of dominating pores performed a transversal amplification from barrier-type layer to pore structure. The pore cells were perpendicular with column constriction near the second-phase particles and parallelism with the layer growth. Both the barrier-type oxide layer and porous oxide layer perform excellent corrosion protection on aluminium substrate with the corrosion current density of 10-10 A/cm 2 and transfer impedance of 10 7 Ω cm 2. The former leads to the more effective anti-corrosion property.