CN104404597A - Preparation method of porous alpha-alumina membrane - Google Patents
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- 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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- 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
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
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- 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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- 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
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- 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
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- C25D11/18—After-treatment, e.g. pore-sealing
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- 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
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Abstract
A preparation method of a porous alpha-alumina membrane comprises the following steps: carrying out an annealing and electric polishing pretreatment on a high purity aluminum foil; taking the processed aluminum foil as the positive electrode, and graphite as the negative electrode, then carrying out two-step positive electrode oxidation in a mixed solution of phosphoric acid and aluminum oxalate to obtain an aluminum-base-containing porous anodic alumina membrane; subjecting the obtained aluminum-base-containing porous anodic aluminum membrane to a pore enlarging treatment; then subjecting the pore-enlarged aluminum-base-containing porous anodic alumina membrane to a water boiling treatment or a hydrothermal treatment; then removing the aluminum base from the aluminum-base-containing porous anodic alumina membrane, which has been treated by water boiling or a hydrothermal treatment; using a sodium citrate solution to remove the baffle layer and alumina hydrate on the external layer of the porous alumina membrane from the aluminum-base-free porous anodic alumina membrane so as to form a periodical hexahedral densely-arranged alumina through hole structure finally; and sintering the prepared alumina membrane with a periodical hexahedral densely-arranged alumina through hole structure in a muffle furnace at a high temperature so as to obtain porous alpha-alumina membrane.
Description
Technical field
The present invention relates to nanometer synthesis and nanometer technique field, specifically a kind of preparation method with periodically six side's solid matter through-hole structure alpha-alumina inorganic membranes.
Background technology
Due to the thing phase that Alpha-alumina is the most stable in all aluminum oxide, there is the features such as fusing point is high, chemical stability is excellent, therefore alpha-alumina inorganic membrane there is extensive use comprising assemble nanometer material, filtration and be separated in numerous areas.Different methods can be adopted prepare according to the difference of the factor such as membrane pore size, material preparing in alpha-alumina inorganic membrane process.Common methods has solid particles sintering process (dip-coating), anonizing, extension molecular sieve, molecular self-assembling, the methods such as laser ablation.
The well-regulated vesicular structure of porous anodic alumina films tool utilizing anonizing to prepare, in accurate periodically six side's solid matters, cylindricality duct is parallel to each other, and aperture is adjustable on a large scale, the mineral membrane that the vesicular structure of this uniqueness makes multiaperture pellumina become desirable.But, the composition of the multiaperture pellumina prepared owing to utilizing anonizing is mainly by the aluminum oxide of amorphous and the hydrate of aluminum oxide: alumina trihydrate (i.e. aluminium hydroxide) is formed, a large amount of dehydration is caused the curling or cracking of macroscopically diaphragm by the hydrate that this kind of ingredient properties determines porous anodic alumina films at high temperature aluminum oxide, and periodicity six side close-packed configuration orderly on microcosmic is destroyed.Report that this phenomenon is in 1972 the earliest, the people such as Neufeld was (see document P.Neufeld at that time, N.K.Nagpaul, R.Ashdown, and M.Akbar, Electrochimica Acta 17,1972,1543) find that porous anodic alumina films is can undergo phase transition and adjoint shrinkage phenomenon in heating.2006, the people such as I.W.M.Brown are (see document I.W.M.Brown, M.E.Bownden, T.Kemmitt, and K.J.D. MacKenzie, Current Applied Physics 6,2006,557.) carry out detailed analysis to porous anodic alumina films thermal treatment, think when porous anodic alumina films is heated to 850 DEG C, its meeting is curling or cracking under internal mechanical stresses effect.Above document shows to become a worldwide technological puzzle by sintered porous anodised aluminium film preparation alpha-alumina inorganic membrane.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of porous Alpha-alumina film, simple to operate, and efficiently solves the difficulty of prior art existence.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of preparation method of porous Alpha-alumina film, is characterized in that, comprise the steps:
(1) high-purity aluminum foil is annealed, electropolishing pre-treatment;
(2) using step (1) pretreated aluminium foil as anode, take graphite as negative electrode, in phosphoric acid, oxalic acid aluminium mixing solutions, carry out two-step approach anodic oxidation obtain being with aluminium-based porous anodic alumina films;
(3) the aluminium-based porous anodic alumina films of band prepared by step (2) is carried out expanding treatment;
(4) the aluminium-based porous anodic alumina films of band after step (3) expanding treatment is carried out poach or hydrothermal treatment consists;
(5) the aluminium-based porous anodic alumina films of band after step (4) poach or hydrothermal treatment consists is removed aluminium base;
(6) step (5) being removed aluminium base porous anodic alumina films utilizes sodium citrate solution to remove blocking layer and porous alumina outer oxide aluminium hydrate, the final aluminum oxide through-hole structure forming periodically six side's solid matters;
(7) pellumina prepared by step (6) with periodically six side's solid matter through-hole structures is put into retort furnace and carry out high temperature sintering, prepare porous Alpha-alumina film.
As improvement, in described step (1), the purity of described high-purity aluminum foil is more than 99.99%.
As improvement, in described step (1), put into retort furnace and anneal, to eliminate aluminium foil internal stress; Aluminium foil after annealing is ultrasonic cleaning in acetone and ethanol solution respectively, to remove surperficial grease; Then the aluminium foil after cleaning is put into perchloric acid dehydrated alcohol mixed solution and carry out electropolishing under 21V constant voltage.
As improvement, in the electrolytic solution that in described step (2), two-step approach anodic oxidation uses, phosphoric acid quality is than being 0.01-5%, and oxalic acid aluminum concentration is 0.005-0.05 mol/L, and anodic oxidation voltage is 180V-250V, electrolyte temperature is 0-10 DEG C, and the anodised time is 6-24 hour.
As improvement, in described step (3) with mass ratio be 5% phosphoric acid solution for reaming liquid, reaming liquid temp is 10-30 DEG C, and pore-enlargement is 1-5 hour.
As improvement, in described step (4), poach temperature is 80 DEG C-100 DEG C, and hydrothermal temperature is 100 DEG C-150 DEG C, and poach or hydrothermal conditions are 1-10 hour.
As improvement, in described step (6), the concentration of sodium citrate solution is 0.01-0.2 mol/L, and solution temperature is 30 DEG C-100 DEG C, and removal blocking layer and outer oxide aluminium hydrate treatment time are 20-160 minutes.
As improvement, in described step (7), sintering temperature is 1000 DEG C-1600 DEG C, and sintering time is 3-12 hour.
As improvement, the porous anodic alumina films finally obtained, its pitch of holes reaches 530nm, and aperture is homogeneous, and in order, hole density is high in arrangement.
The beneficial effect that the present invention is compared with prior art brought is:
(1) the present invention utilizes phosphoric acid-oxalic acid aluminium mixing solutions to prepare wide aperture porous anodic alumina films, and the preparation-obtained porous anodic alumina films pitch of holes of this inventive method reaches 530nm, and aperture is homogeneous, and in order, hole density is high in arrangement.For the applied research of expansion porous anodic alumina films, the technical progress promoting this area is significant;
(2) the present invention prepares the aluminum oxide inner framework of high-sequential six side solid matter through-hole structure.This inventive method utilizes poach or hydrothermal method to coordinate sodium citrate solution to dissolve and is peeled off by porous anodic alumina films ectonexine, then utilizes sodium citrate solution to dissolve porous anodic aluminium oxide blocking layer and outer oxide aluminium hydrate.Simple, the effective and prepared aluminum oxide inner framework of this method has six side's close-packed configuration of high-sequential, has wide application prospects in assemble nanometer material, filtration and being separated in numerous areas;
(3) the present invention prepares the nanohole alumine mineral membrane of the periodicity six side solid matter with α phase.This invention prepares six side's close-packed configuration porous alpha-alumina inorganic membrane microcosmic with high-sequential, and pitch of holes reaches 530nm, and macroscopically diaphragm is smooth, without any curling or cracking phenomena.Fundamentally solve and utilize porous anodic alumina films to prepare this technical barrier of alpha-alumina inorganic membrane through oversintering.
Accompanying drawing explanation
Fig. 1 is that the pellumina SEM of periodically six side's solid matter through-hole structures schemes.
Fig. 2 is 1300 DEG C of sintering lower preparation porous alpha-alumina inorganic membrane SEM figure.
Fig. 3 is 1300 DEG C of sintering lower preparation porous alpha-alumina inorganic membrane XRD figure.
Fig. 4 is 1400 DEG C of sintering lower preparation porous alpha-alumina inorganic membrane XRD figure.
Embodiment
Below in conjunction with Figure of description, the invention will be further described.
Embodiment 1
A preparation method for porous Alpha-alumina film, comprises the steps:
(1) adopt routine techniques the high-purity aluminum foil that purity is more than 99.99% is annealed, electropolishing pre-treatment; Put into retort furnace to anneal, to eliminate aluminium foil internal stress; Aluminium foil after annealing is ultrasonic cleaning in acetone and ethanol solution respectively, to remove surperficial grease; Then the aluminium foil after cleaning is put into perchloric acid dehydrated alcohol mixed solution and carry out electropolishing under 21V constant voltage;
(2) using step (1) pretreated aluminium foil as anode, take graphite as negative electrode, in phosphoric acid, oxalic acid aluminium mixing solutions, carry out two-step approach anodic oxidation obtain being with aluminium-based porous anodic alumina films; In the electrolytic solution that two-step approach anodic oxidation uses, phosphoric acid quality is than being 0.01-5%, and oxalic acid aluminum concentration is 0.005-0.05 mol/L, and anodic oxidation voltage is 180V-250V, and electrolyte temperature is 0-10 DEG C, and the anodised time is 6-24 hour;
(3) the aluminium-based porous anodic alumina films of band prepared by step (2) is carried out expanding treatment; With mass ratio be 5% phosphoric acid solution for reaming liquid, reaming liquid temp is 10-30 DEG C, and pore-enlargement is 1-5 hour;
(4) the aluminium-based porous anodic alumina films of band after step (3) expanding treatment is carried out poach or hydrothermal treatment consists; Poach temperature is 80 DEG C-100 DEG C, and hydrothermal temperature is 100 DEG C-150 DEG C, and poach or hydrothermal conditions are 1-10 hour;
(5) routine techniques is utilized by the aluminium-based porous anodic alumina films of band after step (4) poach or hydrothermal treatment consists to remove aluminium base;
(6) step (5) being removed aluminium base porous anodic alumina films utilizes sodium citrate solution to remove blocking layer and porous alumina outer oxide aluminium hydrate, the final aluminum oxide through-hole structure forming periodically six side's solid matters; The concentration of sodium citrate solution is 0.01-0.2 mol/L, and solution temperature is 30 DEG C-100 DEG C, and removal blocking layer and outer oxide aluminium hydrate treatment time are 20-160 minutes;
(7) pellumina prepared by step (6) with periodically six side's solid matter through-hole structures is put into retort furnace and carry out high temperature sintering, middle sintering temperature is 1000 DEG C-1600 DEG C, and sintering time is 3-12 hour; Prepare porous Alpha-alumina film, its pitch of holes reaches 530nm, and aperture is homogeneous, and in order, hole density is high in arrangement.
Embodiment 2
A preparation method for porous Alpha-alumina film, comprises the steps:
(1) high-purity aluminum foil (purity more than 99.99%) to be put at retort furnace 450 DEG C annealing 6 hours, to eliminate aluminium foil internal stress, the ultrasonic cleaning 15 minutes in acetone and ethanol solution respectively of the aluminium foil after annealing, to remove surperficial grease; Then the perchloric acid dehydrated alcohol mixed solution aluminium foil after cleaning being put into volume ratio 1:4 carries out electropolishing under 21V constant voltage;
(2) using step (1) pretreated aluminium foil as anode, take graphite as negative electrode, in mass ratio is 1% phosphoric acid and 0.01 mol/L oxalic acid aluminium mixing solutions, carries out two-step approach anodic oxidation; Anodic oxidation voltage is 210V, and electrolyte temperature is 5 DEG C, and the anodised time is 8 hours;
(3) the aluminium-based porous anodic alumina films of band prepared by step (2) with mass ratio be 5% phosphoric acid solution for reaming liquid, reaming liquid temp is 20 DEG C, and pore-enlargement is 2 hours, carries out expanding treatment;
(4) the aluminium-based porous anodic alumina films of band after step (3) expanding treatment is carried out poach process, temperature is 100 DEG C, and the time is 5 hours;
(5) saturated Cupric Chloride Solution is utilized by the aluminium-based porous anodic alumina films of band after step (4) 100 DEG C of poach process to remove aluminium base;
(6) step (5) being removed aluminium base porous anodic alumina films soaking temperature is 80 DEG C, 0.08 mol/L sodium citrate solution, soak time is 80 minutes, to remove blocking layer and outer aluminium sesquioxide hydrate, prepare the pellumina with periodically six side's solid matter through-hole structures, stereoscan photograph as shown in Figure 1;
(7) pellumina prepared by step (6) with periodically six side's solid matter through-hole structures is put into retort furnace and sinter 5 hours at temperature is 1300 DEG C, prepare porous alpha-alumina inorganic membrane, as shown in Figure 2, XRD figure spectrum as shown in Figure 3 for stereoscan photograph.
Embodiment 3:
The present embodiment is implemented under following technical requirements condition:
In the present embodiment, other condition is identical with embodiment 2.Using step (1) pretreated aluminium foil as anode, take graphite as negative electrode, in mass ratio is 0.03% phosphoric acid and 0.005 mol/L oxalic acid aluminium mixing solutions, carries out two-step approach anodic oxidation.Anodic oxidation voltage is 185V, and electrolyte temperature is 0 DEG C, and the anodised time is 10 hours.Implement the porous alpha-alumina inorganic membrane that above method finally prepares periodically six side's solid matter through-hole structures.
Embodiment 4:
The present embodiment is implemented under following technical requirements condition:
In the present embodiment, other condition is identical with embodiment 2.The aluminium-based porous anodic alumina films of band prepared by step (2) with mass ratio be 5% phosphoric acid solution for reaming liquid, reaming liquid temp is 10 DEG C, and pore-enlargement is 5 hours, carries out expanding treatment.Implement the porous alpha-alumina inorganic membrane that above method finally prepares periodically six side's solid matter through-hole structures.
Embodiment 5:
The present embodiment is implemented under following technical requirements condition:
In the present embodiment, other condition is identical with embodiment 2.The aluminium-based porous anodic alumina films of band after step (3) expanding treatment is carried out hydrothermal treatment consists, and temperature is 120 DEG C, and the time is 3 hours.Implement the porous alpha-alumina inorganic membrane that above method finally prepares periodically six side's solid matter through-hole structures.
Embodiment 6:
The present embodiment is implemented under following technical requirements condition:
In the present embodiment, other condition is identical with embodiment 2.It is 50 DEG C that step (5) is removed aluminium base porous anodic alumina films soaking temperature, 0.02 mol/L sodium citrate solution, and soak time is 140 minutes, to remove blocking layer and outer aluminium sesquioxide hydrate.Implement the porous alpha-alumina inorganic membrane that above method finally prepares periodically six side's solid matter through-hole structures.
Embodiment 7:
The present embodiment is implemented under following technical requirements condition:
In the present embodiment, other condition is identical with embodiment 2.The pellumina prepared by step (6) with periodically six side's solid matter through-hole structures is put into retort furnace at temperature is 1400 DEG C, sinters 5 hours, prepare porous alpha-alumina inorganic membrane.XRD figure spectrum as shown in Figure 4.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. a preparation method for porous Alpha-alumina film, is characterized in that, comprises the steps:
High-purity aluminum foil is annealed, electropolishing pre-treatment;
Using step (1) pretreated aluminium foil as anode, take graphite as negative electrode, in phosphoric acid, oxalic acid aluminium mixing solutions, carry out two-step approach anodic oxidation obtain being with aluminium-based porous anodic alumina films;
The aluminium-based porous anodic alumina films of band step (2) prepared carries out expanding treatment;
The aluminium-based porous anodic alumina films of band after step (3) expanding treatment is carried out poach or hydrothermal treatment consists;
The aluminium-based porous anodic alumina films of band after step (4) poach or hydrothermal treatment consists is removed aluminium base;
Step (5) being removed aluminium base porous anodic alumina films utilizes sodium citrate solution to remove blocking layer and porous alumina outer oxide aluminium hydrate, the final aluminum oxide through-hole structure forming periodically six side's solid matters;
The pellumina prepared by step (6) with periodically six side's solid matter through-hole structures is put into retort furnace and carries out high temperature sintering, prepare porous Alpha-alumina film.
2. the preparation method of a kind of porous Alpha-alumina film according to claim 1, is characterized in that: in described step (1), and the purity of described high-purity aluminum foil is more than 99.99%.
3. the preparation method of a kind of porous Alpha-alumina film according to claim 1, is characterized in that: in described step (1), put into retort furnace and anneal, to eliminate aluminium foil internal stress; Aluminium foil after annealing is ultrasonic cleaning in acetone and ethanol solution respectively, to remove surperficial grease; Then the aluminium foil after cleaning is put into perchloric acid dehydrated alcohol mixed solution and carry out electropolishing under 21V constant voltage.
4. the preparation method of a kind of porous Alpha-alumina film according to claim 1, it is characterized in that: in the electrolytic solution that two-step approach anodic oxidation uses in described step (2), phosphoric acid quality is than being 0.01-5%, oxalic acid aluminum concentration is 0.005-0.05 mol/L, anodic oxidation voltage is 180V-250V, electrolyte temperature is 0-10 DEG C, and the anodised time is 6-24 hour.
5. the preparation method of a kind of porous Alpha-alumina film according to claim 1, is characterized in that: in described step (3) with mass ratio be 5% phosphoric acid solution for reaming liquid, reaming liquid temp is 10-30 DEG C, and pore-enlargement is 1-5 hour.
6. the preparation method of a kind of porous Alpha-alumina film according to claim 1, is characterized in that: in described step (4), poach temperature is 80 DEG C-100 DEG C, and hydrothermal temperature is 100 DEG C-150 DEG C, and poach or hydrothermal conditions are 1-10 hour.
7. the preparation method of a kind of porous Alpha-alumina film according to claim 1, it is characterized in that: in described step (6), the concentration of sodium citrate solution is 0.01-0.2 mol/L, solution temperature is 30 DEG C-100 DEG C, and removal blocking layer and outer oxide aluminium hydrate treatment time are 20-160 minutes.
8. the preparation method of a kind of porous Alpha-alumina film according to claim 1, is characterized in that: in described step (7), sintering temperature is 1000 DEG C-1600 DEG C, and sintering time is 3-12 hour.
9. the preparation method of a kind of porous Alpha-alumina film according to claim 1, it is characterized in that: the porous anodic alumina films finally obtained, its pitch of holes reaches 530nm, and aperture is homogeneous, and in order, hole density is high in arrangement.
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| CN105734638A (en) * | 2016-04-05 | 2016-07-06 | 新乡学院 | Method for preparing aluminum oxide crystalline substrate through anodic oxidation |
| CN107243362A (en) * | 2017-06-07 | 2017-10-13 | 南京工业大学 | Non-coating metal matrix monolithic catalyst carrier/catalyst based on anodic alumina modification and preparation method thereof |
| CN107502936A (en) * | 2017-08-04 | 2017-12-22 | 西北工业大学 | A kind of method for obtaining large aperture doubled via AAO films |
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| CN112391659A (en) * | 2019-08-14 | 2021-02-23 | 浙江苏泊尔股份有限公司 | Method for preparing oxide film containing alpha-alumina and vessel |
| CN113355712A (en) * | 2021-05-14 | 2021-09-07 | 张健 | Preparation method of corrosion-resistant aluminum alloy |
| CN113388873A (en) * | 2021-04-25 | 2021-09-14 | 中国科学院福建物质结构研究所 | Flaky alumina and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110208304A (en) * | 2019-06-17 | 2019-09-06 | 新疆众和股份有限公司 | A kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance |
| CN112391659A (en) * | 2019-08-14 | 2021-02-23 | 浙江苏泊尔股份有限公司 | Method for preparing oxide film containing alpha-alumina and vessel |
| CN113388873A (en) * | 2021-04-25 | 2021-09-14 | 中国科学院福建物质结构研究所 | Flaky alumina and preparation method and application thereof |
| CN113355712A (en) * | 2021-05-14 | 2021-09-07 | 张健 | Preparation method of corrosion-resistant aluminum alloy |
| CN113355712B (en) * | 2021-05-14 | 2024-12-13 | 兴发新材(浙江)有限公司 | A method for preparing corrosion-resistant aluminum alloy |
| CN114497435A (en) * | 2022-01-21 | 2022-05-13 | 西安交通大学 | A kind of aluminum battery negative electrode and its anodic oxidation preparation method and application |
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