Method for efficiently preparing nano material by using anodic aluminum oxide template

Abstract

The invention discloses a method for efficiently preparing a nano material by using an anodic aluminum oxide template, which comprises the following steps: S1, carrying out surface pretreatment on an aluminum foil to ensure that the surface of the aluminum foil is clean and flat; s2, the pretreated aluminum foil is placed in electrolyte, primary anodic oxidation is carried out under the constant current density, and an aluminum oxide film with a certain thickness is formed; s3, removing the barrier layer formed by primary oxidation by using a specific chemical solution; s4, anodic oxidation is conducted again under the same electrolyte condition, pores are further expanded, and a more regular nanometer pore channel structure is formed; s5, filling the target nano material into the pore channels of the anodic aluminum oxide template by adopting a direct-current electrodeposition mode; and S6, the anodic aluminum oxide template is removed through a physical means, and the nanometer material with the highly-ordered structure is released. According to the preparation method, the preparation efficiency and quality of the nano material can be remarkably improved, and the preparation method has important value especially for application occasions needing highly ordered structures.

Description

Technical Field

[0001] The invention relates to the technical field of nano material preparation, and in particular to a method for efficiently preparing nano material by utilizing an anodic aluminum oxide template. Background Art

[0002] Nanomaterials have shown broad application prospects in electronics, optics, biomedicine and other fields due to their unique physical and chemical properties. As an important tool for preparing nanostructures, anodized aluminum oxide (AAO) templates are widely used due to their advantages such as uniform pore size and controllable pore depth. However, the existing AAO template preparation methods have some defects, such as uneven pore size distribution and easy pore blockage. These problems not only affect the performance of nanomaterials, but also limit their use in applications that require highly ordered structures.

[0003] In addition, the traditional method has low preparation efficiency and is difficult to meet the needs of large-scale industrial production. Therefore, it is particularly urgent to develop a new method that can overcome the above problems and improve the quality and production efficiency of nanomaterials. Summary of the invention

[0004] 1. Technical Problems Solved The technical problems to be solved by the present invention are the various problems mentioned in the above background technology, and a method for efficiently preparing nanomaterials using an anodic aluminum oxide template is provided. Technical Solution

[0005] In order to solve the above technical problems, the present invention provides a technical solution: a method for efficiently preparing nanomaterials using an anodic aluminum oxide template, comprising the following steps: S1. Pre-treat the surface of the aluminum foil to ensure that the surface of the aluminum foil is clean and smooth; S2, placing the pretreated aluminum foil in an electrolyte, and performing primary anodization at a constant current density to form an aluminum oxide film with a certain thickness; S3, using a specific chemical solution to remove the barrier layer formed by the primary oxidation; S4, anodizing again under the same electrolyte conditions to further expand the pores and form a more regular nanopore structure; S5, using direct current electrodeposition to fill the target nanomaterial into the pores of the anodized aluminum template; S6. Remove the anodized aluminum template by physical means to release nanomaterials with highly ordered structures.

[0006] As an improvement, the surface pretreatment includes degreasing and chemical polishing to ensure the cleanliness and flatness of the aluminum foil surface.

[0007] As an improvement, during the primary anodization process, the thickness and pore size of the film can be adjusted by precisely controlling the electrolysis conditions, which include voltage, temperature and time.

[0008] As an improvement, the chemical solution used to remove the barrier layer formed by primary oxidation includes an acid etchant of phosphoric acid and chromic acid.

[0009] As an improvement, the same electrolyte conditions as those of the initial anodization are used during the secondary anodization process to ensure the consistency and regularity of the nanopore structure.

[0010] As an improvement, the physical means of removing the anodized aluminum template includes ultrasonic vibration treatment and heat treatment, so as to remove the anodized aluminum template. Beneficial Effects

[0011] The advantages of the present invention compared with the prior art are: The present invention provides a method for efficiently preparing nanomaterials using anodized aluminum templates, which achieves high controllability of nanopore size and distribution through optimized surface pretreatment, precisely controlled primary anodization, barrier layer removal, secondary anodization, direct current electrodeposition, and physical removal of templates, effectively avoiding pore blockage and enhancing the regularity and consistency of the pores. This method can not only significantly improve the preparation efficiency and quality of nanomaterials, especially for applications requiring highly ordered structures, but also is simple to operate, low in cost, and easy to achieve large-scale industrial production, providing strong technical support for the development of nanotechnology. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 The present invention is a flow chart of the steps of a method for efficiently preparing nanomaterials using an anodic aluminum oxide template. DETAILED DESCRIPTION

[0013] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention. Example

[0014] like Figure 1 As shown, a method for efficiently preparing nanomaterials using an anodic aluminum oxide template comprises the following steps: S1. Pre-treat the surface of the aluminum foil to ensure that the surface of the aluminum foil is clean and smooth; S2, placing the pretreated aluminum foil in an electrolyte, and performing primary anodization at a constant current density to form an aluminum oxide film with a certain thickness; S3, using a specific chemical solution to remove the barrier layer formed by the primary oxidation; S4, anodizing again under the same electrolyte conditions to further expand the pores and form a more regular nanopore structure; S5, using direct current electrodeposition to fill the target nanomaterial into the pores of the anodized aluminum template; S6. Remove the anodized aluminum template by physical means to release nanomaterials with highly ordered structures.

[0015] Specifically, the surface pretreatment includes degreasing and chemical polishing to ensure the cleanliness and flatness of the aluminum foil surface. During the initial anodizing process, the thickness and pore size of the film can be adjusted by precisely controlling the electrolysis conditions, and the electrolysis conditions include voltage, temperature and time. The chemical solution used to remove the barrier layer formed by the initial oxidation includes acid corrosive agents such as phosphoric acid and chromic acid. During the secondary anodizing process, the same electrolyte conditions as those of the initial anodizing are used to ensure the consistency and regularity of the nanopore structure. The physical means of removing the anodized aluminum template include ultrasonic vibration treatment and heat treatment to remove the anodized aluminum template.

[0016] The specific implementation process of the present invention is as follows: Surface pretreatment: Select pure aluminum foil with a thickness of about 0.5 mm. First, degrease and deoil it by immersing it in a mixed solution containing NaOH and Na2CO3. The temperature is controlled at 70-80°C. The immersion time is 10 minutes, and then it is cleaned with deionized water. Then, chemical polishing is performed by immersing the aluminum foil in a polishing solution composed of HNO3 and H2O. The temperature is controlled at room temperature. The immersion time is 5 minutes, and then it is thoroughly cleaned with deionized water to ensure that the surface of the aluminum foil is clean and flat.

[0017] Initial anodization: The pretreated aluminum foil is fixed at the anode position and immersed in a 0.3 M oxalic acid solution. The constant current density is set to 0.15 A / cm², the temperature is controlled at 0-5°C, and the oxidation time is 40 hours to form an aluminum oxide film with a certain thickness. The thickness and pore size of the film can be adjusted by precisely controlling the voltage, temperature and time.

[0018] Removal of barrier layer: The aluminum foil after primary oxidation was immersed in a 6 wt% phosphoric acid solution at 40 °C for 30 min to remove the barrier layer formed by primary oxidation and expose the underlying pore structure.

[0019] Secondary anodization: Under the same electrolyte conditions (0.3 M oxalic acid solution, 0.15 A / cm², 0-5°C), anodization was performed again for 60 h to further expand the pores and form a more regular nanoporous structure.

[0020] Nanomaterial filling: The anodized aluminum template after secondary oxidation is used as the working electrode and immersed in an electrolyte containing the target nanomaterial precursor. The target nanomaterial is filled into the pores of the template by direct current deposition with a current density of 0.05 A / cm² and a deposition time of 30 minutes to form a nanowire or nanotube structure.

[0021] Template removal: The anodized aluminum template filled with nanomaterials was immersed in a 5 wt% NaOH solution at 60°C for 1 hour to remove the anodized aluminum template by alkaline corrosion; or the template was placed in an ultrasonic cleaner and subjected to ultrasonic vibration treatment with deionized water for about 30 minutes to physically remove the template and ultimately release the nanomaterial with a highly ordered structure.

[0022] Through the above method, the present invention can significantly improve the preparation efficiency and quality of nanomaterials, especially for applications requiring highly ordered structures. The method is simple to operate, low in cost, and easy to achieve large-scale industrial production, providing strong technical support for the development of nanotechnology.

[0023] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0024] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

[0025] The present invention and its embodiments are described above, and such description is not restrictive. The drawings show only one embodiment of the present invention, and the actual structure is not limited thereto. In short, if ordinary technicians in the field are inspired by it, without departing from the purpose of the invention, they can design a structure and embodiment similar to the technical solution without creativity, which should belong to the protection scope of the present invention.

Claims

1. A method for efficiently preparing nanomaterials using anodized aluminum templates, characterized in that: The following steps are involved: S1. Pre-treat the surface of the aluminum foil to ensure that the surface of the aluminum foil is clean and smooth; S2, placing the pretreated aluminum foil in an electrolyte, and performing primary anodization at a constant current density to form an aluminum oxide film with a certain thickness; S3, using a specific chemical solution to remove the barrier layer formed by the primary oxidation; S4, anodizing again under the same electrolyte conditions to further expand the pores and form a more regular nanopore structure; S5, using direct current electrodeposition to fill the target nanomaterial into the pores of the anodized aluminum template; S6. Remove the anodized aluminum template by physical means to release nanomaterials with highly ordered structures.

2. The method for efficiently preparing nanomaterials using anodized aluminum templates according to claim 1, characterized in that: The surface pretreatment includes degreasing and chemical polishing to ensure the cleanliness and flatness of the aluminum foil surface.

3. The method for efficiently preparing nanomaterials using an anodic aluminum oxide template according to claim 1, characterized in that: During the primary anodization process, the thickness and pore size of the film can be adjusted by precisely controlling the electrolysis conditions, which include voltage, temperature and time.

4. The method for efficiently preparing nanomaterials using anodized aluminum templates according to claim 1, characterized in that: The chemical solution used to remove the barrier layer formed by primary oxidation includes an acid etchant of phosphoric acid and chromic acid.

5. The method for efficiently preparing nanomaterials using anodized aluminum templates according to claim 1, characterized in that: During the secondary anodization process, the same electrolyte conditions as those of the primary anodization are used to ensure the consistency and regularity of the nanopore structure.

6. The method for efficiently preparing nanomaterials using anodized aluminum templates according to claim 1, characterized in that: The physical means for removing the anodized aluminum template includes ultrasonic vibration treatment and heat treatment, thereby removing the anodized aluminum template.

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