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Electrochemical method for detecting anodic oxidation aluminium formwork effective hole density

An anodized aluminum, electrochemical technology, applied in the direction of material electrochemical variables, measuring devices, scientific instruments, etc., can solve problems such as failure, inability to function, blind holes cannot be excluded, and achieve the effect of simple method and good reliability

Inactive Publication Date: 2007-06-27
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Usually, the pore density (porosity) of the AAO template is obtained by observing the scanning electron microscope (SEM) or the atomic force microscope (AFM). The problem is that some holes may be "blind holes" that are not connected, and are obtained by SEM or AFM testing. It is only the apparent hole density. "Blind holes" cannot play a role in the preparation of nanowires in electrodeposition experiments, and the tests of SEM or AFM cannot exclude the "blind holes". However, the determination of the effective hole density of AAO templates has not no report

Method used

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  • Electrochemical method for detecting anodic oxidation aluminium formwork effective hole density
  • Electrochemical method for detecting anodic oxidation aluminium formwork effective hole density
  • Electrochemical method for detecting anodic oxidation aluminium formwork effective hole density

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Embodiment 1

[0015] Embodiment 1: adopt three-electrode system, working electrode is the platinum electrode that self-made AAO template is arranged on the surface of working electrode is metal platinum disc electrode, and reference electrode is saturated calomel electrode (SCE), and counter electrode is platinum wire, and solution is 5mM K 3 Fe(CN) 6 , which contains 0.5M KCl supporting electrolyte. The cyclic voltammogram of the bare electrode (a) after the template exists on the electrode surface (b) is shown in Figure 5, the peak potential decreases from 65mV to 45mV, and the peak current decreases from 1.080×10 -5 A is reduced to 6.718×10 -6 a. Figure 7 is the SEM image of the self-made AAO template. The pore diameter is about 70nm. According to the ratio of the peak current before and after the template exists on the electrode surface and the value of the pore diameter, the pore density of the self-made AAO template can be calculated as 1.61×10 10 piece / cm 2 . This value is in th...

Embodiment 2

[0024] Embodiment 2: A three-electrode system is adopted, the working electrode is a metal platinum disk electrode and a platinum electrode with an AAO template on the surface, the reference electrode is an Ag / AgCl electrode, the counter electrode is a platinum wire, and the solution is 5mM K 3 Fe(CN) 6 , which contains 0.5M Na 2 SO 4 Supports electrolytes. at 5mM K 3 Fe(CN) 6 In the solution, at 10mV / s, 20mV / s, 40mV / s, 60mV / s, 80mV / s, 100mV / s, scan in the potential range from 0 to +0.5V, and record the cyclic voltammogram respectively (Figure 1), The redox peak spacing is about 60mV. When there is a template on the electrode surface, K 3 Fe(CN) 6 The reaction on the electrode is carried out through the pores of AAO, showing a controlled diffusion behavior, and the redox peak distance is about 40mV (Figure 2). At the same time, the peak current decreases, and the peak current still increases with the increase of the scan rate. , and the square root of the peak current ...

Embodiment 3

[0025] Embodiment 3: a three-electrode system is adopted, the working electrode is a metal platinum disk electrode and a platinum electrode with an AAO template on the surface, the reference electrode is an Ag / AgCl electrode, the counter electrode is a platinum wire, and the solution is 1mM K3 Fe(CN) 6 , which contains 0.5M Na 2 SO 4 Supports electrolytes. With 10mV / s, 20mV / s, 40mV / s, 60mV / s, 80mV / s, 100mV / s, scan in the potential range from 0 to +0.5V, record the cyclic voltammogram (Figure 3), redox peak The spacing is about 60mV. When there is a template, K 3 Fe(CN) 6 The reaction on the electrode is carried out through the pores of AAO, and the redox peak distance is less than 60mV (Figure 4). At the same time, the peak current decreases, and the peak current still increases with the increase of the scan rate. Exhibits a good linear relationship. The electrochemical effective area can be obtained from the slope of the straight line. Further, the effective pore densi...

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Abstract

The invention especially related to electrochemical method for measuring effective density of hole in anodic aluminum oxide (AAO) template. Usual three-electrode system and potentiostat are adopted in the method. Working electrode is dish electrode of metal platinum (or gold, glassy carbon), and there is electrode of AAO template. Ferricyanide is as solution. Na2SO4 or KCl is as electrolyte. Using diffusibility of ferricyanide on surface of working electrode, the method measures effective density of hole in AAO template by using electrochemical voltmeter-ammeter method. Features are: simple method and good reliability.

Description

technical field [0001] The invention belongs to the technical field of nanometer detection, and specifically relates to a method for measuring the effective pore density (the ratio of the total area of ​​pores to the total geometric area) and porosity (the number of pores per unit geometric area) of an anodized aluminum template by electrochemical cyclic voltammetry new method. Background technique [0002] Anodic aluminum oxide template (Anodic Aluminum Oxide, AAO) is one of the most commonly used templates for the preparation of nanomaterials, and plays a very important role in the field of nanoscience and technology. The diameter can be controlled by selecting the concentration and type of acid and the anodizing voltage, and the thickness of the film depends on the time of anodizing. Synthesis of nanostructure units and nanostructure array systems by template method is a cutting-edge technology developed in the 1990s. It is an integration of multiple physical and chemica...

Claims

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Application Information

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IPC IPC(8): G01N15/08G01N27/48
Inventor 崔晓莉赵强李志州孙子颖江志裕
Owner FUDAN UNIV
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