CN111485268A - Preparation method for rapidly preparing alumina template by using 1060 aluminum sheet at high temperature - Google Patents
Preparation method for rapidly preparing alumina template by using 1060 aluminum sheet at high temperature Download PDFInfo
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- CN111485268A CN111485268A CN202010306971.4A CN202010306971A CN111485268A CN 111485268 A CN111485268 A CN 111485268A CN 202010306971 A CN202010306971 A CN 202010306971A CN 111485268 A CN111485268 A CN 111485268A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/12—Anodising more than once, e.g. in different baths
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
Abstract
The invention relates to a preparation method for rapidly preparing an aluminum oxide template at high temperature by using a 1060 aluminum sheet, which relates to the technical field of preparation of the aluminum oxide template, in particular to a preparation method for rapidly preparing the aluminum oxide template at 28 ℃ by using the 1060 aluminum sheet with the purity of 99.6 percent, wherein the preparation method comprises the steps of carrying out high-temperature annealing, ultrasonic cleaning and electrochemical polishing on the aluminum sheet, carrying out anodic oxidation on the aluminum sheet by using a treated aluminum sheet as an anode and a millstone rod as a cathode in a 0.3 mol/L sulfuric acid solution at 28 ℃ for 1 hour at the voltage of 20V or 25V, removing oxygen, soaking the aluminum sheet in a mixed solution of 1.8 percent of chromic acid and 6 percent of phosphoric acid at the temperature of 60 ℃ for 1.5 hours to remove an oxidation film, and carrying out re-oxidation treatment on the aluminum sheet by using the millstone rod as the anode and anodizing in a 0.3 mol/L sulfuric acid solution at the temperature of 28 ℃ for 1 hour, 2 hours or 3 hours at the voltage of 20V.
Description
Technical Field
The invention discloses a preparation method for rapidly preparing an alumina template by using 1060 aluminum sheets at a high temperature, relates to the technical field of alumina template preparation, and particularly relates to a preparation method for using 1060 aluminum sheets with the purity of 99.6% to prepare the alumina template at the temperature of 28 ℃.
Background
At present, the porous anodic alumina template has wide application in the field of synthesis of one-dimensional nano materials due to higher thermodynamic stability and extremely high length-diameter ratio of pore channels. Has a great deal of application in the fields of optics, mechanics, magnetism, medicine and the like. The preparation of alumina templates has been extensively developed over decades of development. The current mainstream methods are a mild oxidation method, a strong oxidation method, a pulse oxidation method, a periodic oxidation method and a mold pressing oxidation method. Secondary oxidation under mild oxidation was mainly used in the laboratory. The preparation process of the alumina template is simplified since the birth of the secondary oxidation preparation method of the alumina template, and the alumina template is developed rapidly. However, the traditional secondary oxidation preparation method needs to prepare the aluminum sheet with the purity of 99.999 percent for 18 to 20 hours at the low temperature of between 0 and 3 ℃. Wherein the temperature condition of 0 ℃ to 3 ℃ is harsh, the aluminum sheet with the purity of 99.999 percent is expensive, and the preparation time is very long. These have severely hampered the large-scale laboratory application of alumina templates.
Aiming at the problems in the prior art, a novel preparation method for rapidly preparing an alumina template by using 1060 aluminum sheets at high temperature is researched and designed, so that the problems in the prior art are very necessary to be overcome.
Disclosure of Invention
According to the technical problems of high price of raw materials, long preparation time and the like in the prior art, the preparation method for rapidly preparing the alumina template by using 1060 aluminum sheets at high temperature is provided. The method mainly selects 1060 aluminum sheet to replace the aluminum sheet with the purity of 99.999, and adopts a secondary anodic oxidation method to prepare the aluminum sheet at the temperature of 28 ℃, thereby achieving the effect of reducing the preparation cost and the preparation time.
The technical means adopted by the invention are as follows:
a method for rapidly preparing an alumina template by using 1060 aluminum sheets at a high temperature comprises the following steps: A. pretreatment, B, anodic oxidation, C, removal of an oxidation film, D and reoxidation treatment;
A. a pretreatment step: carrying out three steps of high-temperature annealing, ultrasonic cleaning and electrochemical polishing on the 1060 aluminum sheet with low purity;
the high-temperature annealing step is to place the aluminum sheet in a tube furnace for high-temperature annealing for 4 hours at the temperature of 500 ℃ under the protection of nitrogen.
The ultrasonic cleaning is firstly carried out for 10 minutes by adopting ethanol, and then is carried out for 10 minutes by adopting deionized water.
The electrochemical polishing takes an aluminum sheet as an anode and stainless steel as a cathode, and the ratio of phosphoric acid to sulfuric acid is 7: 3, the mass fraction of ethylene glycol is 16 percent, and the temperature is 85 ℃ and the concentration is 30A/dm2And (4) performing current density electrochemical polishing.
B. Anodizing, namely anodizing the aluminum sheet pretreated in the step A in a 0.3 mol/L sulfuric acid solution at the temperature of 28 ℃ for 1 hour at the voltage of 20V or 25V by using a stone grinding rod as a cathode;
C. removing an oxidation film: b, immersing the anodized aluminum sheet in the step B into a mixed solution of 1.8% chromic acid and 6% phosphoric acid at 60 ℃, and immersing for 1.5 hours to remove an oxide film;
D. and C, a reoxidation treatment step, namely, taking the aluminum sheet treated in the step C as an anode and a stone grinding rod as a cathode, and anodizing the aluminum sheet for 1 hour, 2 hours or 3 hours in a 0.3 mol/L sulfuric acid solution at the temperature of 28 ℃ under the voltage condition of 20V.
After the four steps of treatment, the excellent alumina template material with smooth and clean surface and orderly pore canal distribution is finally obtained.
Compared with the prior art, the invention has the following advantages:
1. according to the preparation method for rapidly preparing the alumina template at the high temperature by using the 1060 aluminum sheet, the 1060 aluminum sheet is adopted to replace the aluminum sheet with the purity of 99.999 percent, so that the cost of raw materials is reduced;
2. according to the preparation method for rapidly preparing the alumina template at the high temperature by using the 1060 aluminum sheet, the experimental time is only 5.5 hours due to the adoption of the 28 ℃ temperature condition, and the experimental strength is greatly reduced by consuming 18-20 hours compared with the traditional preparation method at the 0-3 ℃ temperature condition.
In conclusion, the technical scheme of the invention solves the problems of high raw material price, long preparation time and the like in the prior art.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a graph comparing two oxidations in example 1 of the present invention;
FIG. 2 is a graph comparing two oxidations in example 2 of the present invention;
FIG. 3 is a graph comparing two oxidations in example 3 of the present invention;
FIG. 4 is a graph comparing two oxidations in example 4 of the present invention;
FIG. 5 is a graph comparing two oxidations in example 5 of the present invention;
FIG. 6 is a graph comparing two oxidations in example 6 of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. Any specific values in all examples shown and discussed herein are to be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
In the description of the present invention, it is to be understood that the orientation or positional relationship indicated by the directional terms such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal" and "top, bottom", etc., are generally based on the orientation or positional relationship shown in the drawings, and are used for convenience of description and simplicity of description only, and in the absence of any contrary indication, these directional terms are not intended to indicate and imply that the device or element so referred to must have a particular orientation or be constructed and operated in a particular orientation, and therefore should not be considered as limiting the scope of the present invention: the terms "inner and outer" refer to the inner and outer relative to the profile of the respective component itself.
Spatially relative terms, such as "above … …," "above … …," "above … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial relationship to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary term "above … …" can include both an orientation of "above … …" and "below … …". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
It should be noted that the terms "first", "second", and the like are used to define the components, and are only used for convenience of distinguishing the corresponding components, and the terms have no special meanings unless otherwise stated, and therefore, the scope of the present invention should not be construed as being limited.
As shown in the figure, the invention provides a preparation method for rapidly preparing an alumina template by using 1060 aluminum sheets at high temperature, which comprises the following steps: A. pretreatment, B, anodic oxidation, C, removal of an oxidation film, D and reoxidation treatment;
A. a pretreatment step: carrying out three steps of high-temperature annealing, ultrasonic cleaning and electrochemical polishing on the 1060 aluminum sheet with low purity;
the high-temperature annealing step is that the aluminum sheet is placed in a tube furnace to be annealed for 4 hours at the high temperature of 500 ℃ under the protection of nitrogen;
ultrasonic cleaning is carried out for 10 minutes by adopting ethanol, and then ultrasonic cleaning is carried out for 10 minutes by adopting deionized water;
the electrochemical polishing takes an aluminum sheet as an anode and stainless steel as a cathode, and the ratio of phosphoric acid to sulfuric acid is 7: 3, the mass fraction of ethylene glycol is 16 percent, and the temperature is 85 ℃ and the concentration is 30A/dm2Current density electrochemical polishing;
B. anodizing, namely anodizing the aluminum sheet pretreated in the step A in a 0.3 mol/L sulfuric acid solution at the temperature of 28 ℃ for 1 hour at the voltage of 20V or 25V by using a stone grinding rod as a cathode;
C. removing an oxidation film: b, immersing the anodized aluminum sheet in the step B into a mixed solution of 1.8% chromic acid and 6% phosphoric acid at 60 ℃, and immersing for 1.5 hours to remove an oxide film;
D. and C, a reoxidation treatment step, namely, taking the aluminum sheet treated in the step C as an anode and a stone grinding rod as a cathode, and anodizing the aluminum sheet for 1 hour, 2 hours or 3 hours in a 0.3 mol/L sulfuric acid solution at the temperature of 28 ℃ under the voltage condition of 20V.
Example 1
As shown in fig. 1, the present invention provides a method for rapidly preparing an alumina template at a high temperature using 1060 aluminum sheets.
3cm by 0.3mm gauge 1060 aluminum sheets were used. Annealing at 500 deg.c for 4 hr in a tubular furnace under the protection of nitrogen. Ultrasonic cleaning with ethanol for 10 min, and ultrasonic cleaning with deionized water for 10 min. Aluminum sheet is used as anode, stainless steel is used as cathode, and the ratio of phosphoric acid to sulfuric acid is 7: 3, the mass fraction of ethylene glycol is 16 percent, and the temperature is 30A/dm at 85 DEG C2Current density electrochemical polishing, using aluminium sheet as anode grinding rod as cathode, anodizing for 1 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 20V, soaking the sample in mixed solution of 1.8% chromic acid and 6% phosphoric acid at 60 deg.C for 1.5 hr, and anodizing for 1 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 20V to obtain alumina template with smooth and clean surface and ordered pore canal distribution.
The diameter of the pore canal of the finished product is about 16nm, and the product can be used as a template material for synthesizing a one-dimensional nano material with high specific surface area and the diameter of about 16nm in a laboratory.
Example 2
As shown in FIG. 2, (on the basis of example 1) the invention also provides a preparation method for rapidly preparing an alumina template at a high temperature by using 1060 aluminum sheets.
3cm by 0.3mm gauge 1060 aluminum sheets were used. Annealing at 500 deg.c for 4 hr in a tubular furnace under the protection of nitrogen. Ultrasonic cleaning with ethanol for 10 min, and ultrasonic cleaning with deionized water for 10 min. Aluminum sheet is used as anode, stainless steel is used as cathode, and the ratio of phosphoric acid to sulfuric acid is 7: 3, the mass fraction of ethylene glycol is 16 percent, and the temperature is 30A/dm at 85 DEG C2Current density electrochemical polishing, using aluminium sheet as anode grinding rod as cathode, anodizing for 1 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 20V, soaking the sample in mixed solution of 1.8% chromic acid and 6% phosphoric acid at 60 deg.C for 1.5 hr, and anodizing for 2 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 20V to obtain alumina template with smooth and clean surface and ordered pore canal distribution.
The diameter of the pore channel of the finished product is about 19nm, and the porous material can be used as a template for synthesizing a one-dimensional nano material with high specific surface area and about 19nm diameter in a laboratory.
Example 3
As shown in fig. 3, (on the basis of example 1) the present invention also provides a preparation method for rapidly preparing an alumina template at a high temperature using 1060 aluminum sheets.
3cm by 0.3mm gauge 1060 aluminum sheets were used. Annealing at 500 deg.c for 4 hr in a tubular furnace under the protection of nitrogen. Ultrasonic cleaning with ethanol for 10 min, and ultrasonic cleaning with deionized water for 10 min. Aluminum sheet is used as anode, stainless steel is used as cathode, and the ratio of phosphoric acid to sulfuric acid is 7: 3, the mass fraction of ethylene glycol is 16 percent, and the temperature is 30A/dm at 85 DEG C2Electrochemical polishing with current density, anodizing the treated aluminum sheet in 0.3 mol/L sulfuric acid solution at 28 deg.c and 20V voltage for 1 hr, and adding 1.8% chromic acid and 6% phosphorusSoaking in acid mixed solution at 60 deg.c for 1.5 hr, and final anode oxidation in 0.3 mol/L sulfuric acid solution at 28 deg.c and 20V for 3 hr to obtain alumina template with smooth and clean surface and ordered pore canal distribution.
The diameter of the pore canal of the finished product is about 22nm, and the finished product can be used as a template for synthesizing a one-dimensional nano material with high specific surface area and about 22nm diameter in a laboratory.
Example 4
As shown in fig. 4, (on the basis of example 1) the present invention also provides a preparation method for rapidly preparing an alumina template at a high temperature using 1060 aluminum sheets.
3cm by 0.3mm gauge 1060 aluminum sheets were used. Annealing at 500 deg.c for 4 hr in a tubular furnace under the protection of nitrogen. Ultrasonic cleaning with ethanol for 10 min, and ultrasonic cleaning with deionized water for 10 min. Aluminum sheet is used as anode, stainless steel is used as cathode, and the ratio of phosphoric acid to sulfuric acid is 7: 3, the mass fraction of ethylene glycol is 16 percent, and the temperature is 30A/dm at 85 DEG C2Current density electrochemical polishing, using aluminium sheet as anode grinding rod as cathode, anodizing for 1 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 25V, soaking the sample in mixed solution of 1.8% chromic acid and 6% phosphoric acid at 60 deg.C for 1.5 hr, and finally anodizing for 1 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 20V to obtain alumina template with smooth and clean surface and ordered pore canal distribution.
The diameter of the pore channel of the finished product is about 17nm, and the finished product can be used as a template for synthesizing a one-dimensional nano material with high specific surface area and the diameter of about 7nm in a laboratory.
Example 5
As shown in fig. 5, (on the basis of example 1) the present invention also provides a preparation method for rapidly preparing an alumina template at a high temperature using 1060 aluminum sheets.
3cm by 0.3mm gauge 1060 aluminum sheets were used. Annealing at 500 deg.c for 4 hr in a tubular furnace under the protection of nitrogen. Ultrasonic cleaning with ethanol for 10 min, and ultrasonic cleaning with deionized water for 10 min. Aluminum sheet is used as anode, stainless steel is used as cathode, and the ratio of phosphoric acid to sulfuric acid is 7: 3B 2Alcohol mass fraction of 16 percent in mixed solution at the temperature of 85 ℃ and the concentration of 30A/dm2Current density electrochemical polishing, using aluminium sheet as anode grinding rod as cathode, anodizing for 1 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 25V, soaking the sample in mixed solution of 1.8% chromic acid and 6% phosphoric acid at 60 deg.C for 1.5 hr, and anodizing for 2 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 20V to obtain alumina template with smooth and clean surface and ordered pore canal distribution.
The diameter of the pore channel of the finished product is about 20nm, and the product can be used as a template for synthesizing a one-dimensional nano material with high specific surface area and the diameter of about 20nm in a laboratory.
Example 6
As shown in fig. 3, (on the basis of example 1) the present invention also provides a preparation method for rapidly preparing an alumina template at a high temperature using 1060 aluminum sheets.
3cm by 0.3mm gauge 1060 aluminum sheets were used. Annealing at 500 deg.c for 4 hr in a tubular furnace under the protection of nitrogen. Ultrasonic cleaning with ethanol for 10 min, and ultrasonic cleaning with deionized water for 10 min. Aluminum sheet is used as anode, stainless steel is used as cathode, and the ratio of phosphoric acid to sulfuric acid is 7: 3, the mass fraction of ethylene glycol is 16 percent, and the temperature is 30A/dm at 85 DEG C2Current density electrochemical polishing, using aluminium sheet as anode grinding rod as cathode, anodizing for 1 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 25V, soaking the sample in mixed solution of 1.8% chromic acid and 6% phosphoric acid at 60 deg.C for 1.5 hr, and finally anodizing for 3 hr in 0.3 mol/L sulfuric acid solution at 28 deg.C and 20V to obtain alumina template with smooth and clean surface and ordered pore canal distribution.
The diameter of the pore canal of the finished product is about 22nm, and the finished product can be used as a template for synthesizing a one-dimensional nano material with high specific surface area and about 22nm diameter in a laboratory.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. The preparation method for rapidly preparing the alumina template by using the 1060 aluminum sheet at a high temperature is characterized by comprising the following steps of: A. pretreatment, B, anodic oxidation, C, removal of an oxidation film, D and reoxidation treatment;
A. a pretreatment step: carrying out three steps of high-temperature annealing, ultrasonic cleaning and electrochemical polishing on an aluminum sheet;
B. anodizing, namely anodizing the aluminum sheet pretreated in the step A in a 0.3 mol/L sulfuric acid solution at the temperature of 28 ℃ for 1 hour at the voltage of 20V or 25V by using a stone grinding rod as a cathode;
C. removing an oxidation film: b, immersing the anodized aluminum sheet in the step B into a mixed solution of 1.8% chromic acid and 6% phosphoric acid at 60 ℃, and immersing for 1.5 hours to remove an oxide film;
D. and C, a reoxidation treatment step, namely, taking the aluminum sheet treated in the step C as an anode and a stone grinding rod as a cathode, and anodizing the aluminum sheet for 1 hour, 2 hours or 3 hours in a 0.3 mol/L sulfuric acid solution at the temperature of 28 ℃ under the voltage condition of 20V.
2. The method for preparing the alumina template using 1060 aluminum sheet high temperature rapid preparation according to claim 1, wherein the high temperature annealing step in the pretreatment step is to place the aluminum sheet in a tube furnace for 500 ℃ high temperature annealing under nitrogen protection for 4 hours.
3. The method of claim 1, wherein the ultrasonic cleaning in the step of pre-treating is performed for 10 minutes by using ethanol and then for 10 minutes by using deionized water.
4. The method of claim 1, wherein the electrochemical polishing step comprises using aluminum sheet as anode, stainless steel as cathode, and performing a high temperature rapid preparation process on the aluminum oxide template with a phosphoric acid/sulfuric acid ratio of 7: 3, the mass fraction of ethylene glycol is 16 percent, and the temperature is 85 ℃ and the concentration is 30A/dm2And (4) performing current density electrochemical polishing.
5. The method for preparing the alumina template using 1060 aluminum sheet high temperature rapid preparation according to claim 1, wherein the aluminum sheet is 1060 aluminum sheet with low purity.
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| CN101298690A (en) * | 2007-05-04 | 2008-11-05 | 特耐固国际有限公司 | Anodizing aluminium and alloys thereof |
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