CN102358948A - Method for preparing anodic alumina template by using plastic packaging process and application thereof - Google Patents
Method for preparing anodic alumina template by using plastic packaging process and application thereof Download PDFInfo
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Abstract
The invention discloses a method for preparing an anodic alumina template by using a plastic packaging process and application thereof. The core point of the method is that the plastic packaging process is utilized for insulation blocking on one surface needing no reaction or treatment of an aluminum sheet, and the method comprises the following steps that: during electrochemical polishing of the aluminum sheet, one surface of the aluminum sheet is sealed by using the plastic packaging process, and the other surface of the aluminum sheet is exposed for polishing; during anodic oxidation of the aluminum sheet, only the surface exposed for polishing is subjected to anodic oxidation due to insulation blocking resulting from plastic packaging; during removal of an aluminum base, by utilizing sealing protection of plastic packaging to the alumina template, a surface of the aluminum base is exposed in a solution and removed so as to obtain the anodic alumina template. The anodic alumina template prepared by the method is colorless and transparent, has a high degree of order and is easy to preserve. According to the invention, high quality alumina templates can be prepared by using plastic package glue cover without any special equipment, and preparation of an alumina template with a large area is made to be simple and easy, thereby greatly improving a success rate of preparing templates, reducing preparation cost for the templates and having remarkable economic benefits.
Description
Technical field
The present invention relates to the electrochemical preparation of template, particularly a kind of method and application that utilizes plastic package process to prepare anodic oxidation aluminium formwork.
Background technology
Template is meant and contains the high-density cylindrical bore that thickness is tens films to the hundreds of micron.Porous alumina formwork is most widely used so far template, and the micropore high-sequential in the film has good thermostability and chemicalstability, is the desirable inorganic template of the uniform sequential nanoelectronic material of preparation shape height.Porous alumina formwork can make through anonizing in acidic solution through rafifinal.This type film have many with the hexagonal array mode arrange, the cylindrical hole of aperture uniformity, be parallel to each other between the duct and perpendicular to the film surface.The bore dia of pellumina is 200 nanometers to the maximum, and minimum is 5 nanometers, and hole density can be up to 10
10Hole/cm
2, film thickness is from 10 microns to 100 microns.
The preparation porous alumina formwork generally adopts the two-step anodization method, and the basic working procedure that obtains the bilateral template comprises: annealing aluminum sheet, electrochemical etching, an anodic oxidation, remove anodic oxide coating, two-step anodization, removal unreacted aluminium base, go to the blocking layer.Experiment is found: factors such as aluminium flake quality, concentration of electrolyte, anodic oxidation temperature, oxidation current density and homogeneity are remarkable to the alumina formwork quality influence.The preparation of alumina formwork generally adopts the single face reaction method to guarantee the specimen preparation quality.At the initial stage, people adopt modes such as insulation grease, sealant tape to realize the single face isolation, but can cause electrolyte contamination; At present; The general single face oxidation of adopting various home-made contrivances to realize aluminium flake; Such as following national inventing patent or the disclosed content of patented claim: publication number CN 101037783A, name is called the national inventing patent application of " utilizing the anodic oxidation bath to prepare the method for orderly anodic oxidation alumina through-hole template "; Publication number 1995480A, name is called the national inventing patent of " preparation technology who obtains the alumina formwork of high-sequential "; Publication number is 1900381A, and name is called the national inventing patent of " preparation facilities of single surface anode aluminum oxide templete "; Publication number is CN 1824844A, and name is called the national inventing patent of " self-supporting bi-pass nano-aluminium oxide form and preparation method thereof "; And publication number is CN 1676676A, and name is called the national inventing patent of " porous aluminium oxide template preparation method and device thereof ", but the common issue with that exists to be tooling cost higher and be difficult to popularize, the low data that cause of standardization level are difficult to use for reference.
Plastic package process is commonly used to sheet articles such as license, data, sample are sealed up for safekeeping and protected, and is easy and simple to handle, with low cost.The main material of plastic packaging film commonly used is polyethylene terephthalate (being called for short PET), its good stability, and transparency is high, oil resistant, anti-diluted acid, diluted alkaline, anti-most of solvents.After changing plastic packaging technology commonly used a little, trial is used for the preparation of anodic oxidation aluminium formwork; If success; With the dependence of breaking away to a great extent preparation facilities; Make low cost, stdn, mass preparation alumina formwork become possibility, the production efficiency in this field is improved have important promoter action.At present, any report or open is not seen in the trial of this direction.
Summary of the invention
The shortcoming that primary and foremost purpose of the present invention is to overcome prior art provides a kind of low cost, the high efficiency method of utilizing plastic package process to prepare anodic oxidation aluminium formwork with not enough.This method can improve the scale and the quality of alumina formwork preparation rapidly, helps the practical application of said material and cost to reduce.
Another object of the present invention is to provide the anodic oxidation aluminium formwork that obtains through the described method of utilizing plastic package process to prepare anodic oxidation aluminium formwork.
A purpose more of the present invention is to provide the described application that utilizes plastic package process to prepare the method for anodic oxidation aluminium formwork.
The object of the invention is realized through following technical proposals: a kind of method of utilizing plastic package process to prepare anodic oxidation aluminium formwork, its core are to utilize the plastic packaging technology with the one side insulation blocking that aluminium flake need not react or handle, and specifically comprise following steps:
(1) in aluminium flake electrochemical etching process, utilize the face seal of plastic packaging to aluminium flake, another side exposes polishing;
(2) in the aluminium flake anode oxidation process,, only carry out anodic oxidation to exposing polished surface because plastic packaging is isolated;
(3) in going aluminium base process, utilize plastic packaging to the alumina formwork seal protection, aluminium base face is exposed in the solution and is removed, and obtains anodic oxidation aluminium formwork.
The described method of utilizing plastic package process to prepare anodic oxidation aluminium formwork more preferably comprises following steps:
(1) cleaning aluminium flake to its surperficial greasy dirt removes;
(2) with cleaned annealing aluminum sheet; The annealing purpose is to increase the grain-size of aluminium flake and reduce the inner mechanical stress of aluminium flake, helps to improve the final film forming degree of order;
(3) aluminium flake of will annealing places the plastic packaging gum cover plastic packaging sealing that a side windows, and the one side that is sealed is not for reacting or handle;
(4) with constant voltage mode the encapsulation aluminium flake is carried out electrochemical etching; Polishing fluid is the absolute ethyl alcohol/perchloric acid mixing solutions of 4: 1 by volume proportionings; Aluminium flake is an anode, and the plastic packaging gum cover is windowed side over against the negative electrode platinized platinum; Polishing voltage 15～20V, 10～15 minutes time; Use magnetic stirring apparatus in the polishing process, make solution temperature and concentration even as far as possible; In the whole polishing process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts; Aluminium flake surface after the polishing is smooth minute surface, and it is residual to remove polishing fluid with washed with de-ionized water;
(5) be anode with the encapsulation aluminium flake, the plastic packaging cover is windowed side over against the negative electrode platinized platinum, carries out an anodic oxidation; Electrolytic solution is the 0.4mol/L oxalic acid solution, and the oxalic acid solution temperature is 4～6 ℃, and voltage constant is 40～50V, and oxidization time is 2～4 hours; In the whole anode oxidation process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts; After oxidation was accomplished, it was residual to remove electrolytic solution with washed with de-ionized water;
(6) the aluminium flake surface after an anodic oxidation has generated multiaperture pellumina; But the degree of order is poor; Need remove the irregular surface that once oxidation forms, only keep the raised grain of distribution uniform, carry out two-step anodization again and just can obtain the pellumina that the degree of order significantly improves; Go the once oxidation film to adopt the mixing solutions of phosphoric acid and chromic acid to soak, wherein phosphoric acid concentration is 6wt%, and chromic acid concentration is 1.8wt%; The mixing solutions temperature of phosphoric acid and chromic acid is 60～65 ℃, soaked 2～4 hours, and magnetic agitation; Whole going in the once oxidation membrane process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts; After soaking end, it is residual to remove solution with washed with de-ionized water;
(7) the same step of condition (5) is carried out two-step anodization to the aluminium flake exposure, and oxidization time is 2～6 hours; In the whole electrolytic process, plastic packaging gum cover good seal; After oxidation was accomplished, it was residual to remove electrolytic solution with washed with de-ionized water;
(8) the plastic packaging gum cover is cut off removal, this moment, aluminium flake simultaneously was the pellumina that behind secondary oxidation, forms, and another side is that unreacted is aluminium base; Be equipped with a same big or small plastic packaging gum cover in addition, a side is opened onesize window, this time with aluminium flake oxidation face package isolation, and aluminium base exposure of unreacted; Aluminium flake behind the plastic packaging is placed saturated Cupric Chloride Solution, expose aluminium base will being removed, the window that a side exposes becomes transparent at this moment; In the whole aluminium flake reaction process, plastic packaging gum cover good seal; After reaction was accomplished, it was residual to remove solution with washed with de-ionized water;
(9) the plastic packaging aluminium flake being placed concentration is that the phosphoric acid solution of 5wt% soaked 40～80 minutes, to remove the alumina formwork blocking layer, must arrive the aperture and be about the bilateral alumina formwork that 60nm, thickness are about 20～60 μ m;
Cleaning described in the step (1) is preferably carried out through following steps: ultrasonic cleaning is 5 minutes in acetone, and behind deionized water rinsing, ultrasonic cleaning is 15 minutes in absolute ethyl alcohol, and is air-dry;
Described ultransonic frequency is preferably 40kHz;
Annealed condition described in the step (2) gets final product by the condition of routine, is preferably 400～500 ℃ of annealing 3～5 hours;
The anodic oxidation aluminium formwork water white transparency that obtains through method for preparing, the degree of order be high, be prone to preserve.
The described method of utilizing plastic package process to prepare anodic oxidation aluminium formwork can be used for the high-quality anodic oxidation aluminium formwork of mass preparation.
The present invention has following advantage and effect with respect to prior art: common plastic packaging machine and plastic packaging gum cover can prepare the effect that main phase such as electrochemical etching in the process, anodic oxidation, aluminium base removal play good single face package isolation at alumina formwork among the present invention; Make method of the present invention not need special device also can prepare high-quality alumina formwork; And make preparation big area alumina formwork also become easily simple; Can improve template widely and be prepared into power; Reduce the template preparation cost, have remarkable economic efficiency.
Description of drawings
Fig. 1 is embodiment 1 prepared alumina formwork stereoscan photograph figure, and wherein: figure A is a vertical view; Figure B is a side elevational view.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
Embodiment 1
(1) with high-purity aluminium flake (purity 99.999%; Beijing Non-ferrous Metal and Rare-earth Application Inst.) be cut into the square of 70 * 50mm, ultrasonic (ultrasonic frequency 40kHz) cleaned 5 minutes in acetone (analytical pure, massfraction is greater than 99.5%); Behind deionized water rinsing; Ultrasonic (ultrasonic frequency 40kHz) cleaned 15 minutes in absolute ethyl alcohol (analytical pure, massfraction is greater than 99.7%), and be air-dry.
(2) aluminium flake is placed box High Temperature Furnaces Heating Apparatus (KSL-1100X, brilliant Materials Technology Ltd. of Hefei section) annealing 5 hours, 500 ℃ of annealing temperatures.
(3) adopt the common rectangular plastic sealing of 95 * 75mm specification cover, and simultaneously cut out 60 * 40mm specification rectangle window at it; The aluminium flake of will annealing places plastic packaging gum cover plastic packaging sealing (F9061 type plastic packaging machine of one mind).
(4) with constant voltage mode the encapsulation aluminium flake is carried out electrochemical etching.Polishing fluid is 4: 1 absolute ethyl alcohol of volume ratio (analytical pure, massfraction is greater than 99.7%), perchloric acid (analytical pure, massfraction is greater than 70.0%) mixing solutions.Aluminium flake is an anode, and the plastic packaging gum cover is windowed side over against the negative electrode platinized platinum.Polishing voltage is chosen as 20V, 15 minutes time.Use magnetic stirring apparatus in the polishing process, make solution temperature and concentration even as far as possible.In the whole polishing process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts.Aluminium flake surface after the polishing is smooth minute surface, and it is residual to remove polishing fluid with deionized water rinsing.
(5) be anode with the encapsulation aluminium flake, the plastic packaging cover is windowed side over against the negative electrode platinized platinum, carries out an anodic oxidation.Electrolytic solution is 0.4mol/L oxalic acid (analytical pure, massfraction is greater than 99.5%) solution, and solution temperature is controlled to be 4～6 ℃, and voltage constant is 45V, oxidization time 2 hours.In the whole electrolytic process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts.After oxidation was accomplished, it was residual to remove electrolytic solution with deionized water rinsing.
(6) go the once oxidation film to adopt phosphoric acid (analytical pure; Massfraction is greater than 85.0%) and chromic acid (analytical pure chromium trioxide; Massfraction is greater than 99.0%) mixing solutions (wherein phosphoric acid concentration is 6wt%, and chromic acid concentration is 1.8wt%) immersion, 60 ℃ of mixing solutions temperature; Soak time 2 hours, and magnetic agitation.Whole going in the once oxidation membrane process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts.After soaking end, it is residual to remove solution with deionized water rinsing.
(7) the same step of condition (5) is carried out two-step anodization to the aluminium flake exposure, and oxidization time is 2 hours.In the whole electrolytic process, plastic packaging gum cover good seal.After oxidation was accomplished, it was residual to remove electrolytic solution with deionized water rinsing.
(8) the plastic packaging gum cover is cut off removal, this moment, aluminium flake simultaneously was the pellumina that behind secondary oxidation, forms, and another side is that unreacted is aluminium base; Be equipped with a same big or small plastic packaging gum cover in addition, a side is opened onesize window, this time with aluminium flake oxidation face package isolation, and aluminium base exposure of unreacted; Aluminium flake behind the plastic packaging is placed saturated cupric chloride (analytical pure, the Copper dichloride dihydrate massfraction is greater than 99.0%) solution, expose aluminium base will being removed, the window that a side exposes becomes transparent at this moment; In the whole aluminium flake reaction process, plastic packaging gum cover good seal; After reaction was accomplished, it was residual to remove solution with deionized water rinsing.
(9) the plastic packaging aluminium flake was placed in 5wt% phosphoric acid (analytical pure, massfraction is greater than the 85.0%) solution 80 minutes, remove the alumina formwork blocking layer, finally obtain the bilateral alumina formwork.In this process, plastic packaging gum cover good seal.
(10) the plastic packaging gum cover is cut off removal, get an amount of template and do the discovery of SEM morphology analysis: the pore size of template distribution range is narrower, is about 60nm; The duct degree of order is higher, is arranged in parallel; Thickness is about 20 μ m (as shown in Figure 1).Because the garment bag protection is nearly all arranged in the whole process of preparation, and it is high to obtain success ratio complete, no damaged alumina formwork.
Embodiment 2
(1) with high-purity aluminium flake (purity 99.999%; Beijing Non-ferrous Metal and Rare-earth Application Inst.) be cut into the square of 70 * 50mm, ultrasonic (ultrasonic frequency 40kHz) cleaned 5 minutes in acetone (analytical pure, massfraction is greater than 99.5%); Behind deionized water rinsing; Ultrasonic (ultrasonic frequency 40kHz) cleaned 15 minutes in absolute ethyl alcohol (analytical pure, massfraction is greater than 99.7%), and be air-dry.
(2) aluminium flake is placed box High Temperature Furnaces Heating Apparatus (KSL-1100X, brilliant Materials Technology Ltd. of Hefei section) annealing 5 hours, 500 ℃ of annealing temperatures.
(3) adopt the common rectangular plastic sealing of 95 * 75mm specification cover, and simultaneously cut out 60 * 40mm specification rectangle window at it; The aluminium flake of will annealing places plastic packaging gum cover plastic packaging sealing (F9061 type plastic packaging machine of one mind).
(4) with constant voltage mode the encapsulation aluminium flake is carried out electrochemical etching.Polishing fluid is 4: 1 absolute ethyl alcohol of volume ratio (analytical pure, massfraction is greater than 99.7%), perchloric acid (analytical pure, massfraction is greater than 70.0%) mixing solutions.Aluminium flake is an anode, and the plastic packaging gum cover is windowed side over against the negative electrode platinized platinum.Polishing voltage is chosen as 20V, 15 minutes time.Use magnetic stirring apparatus in the polishing process, make solution temperature and concentration even as far as possible.In the whole polishing process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts.Aluminium flake surface after the polishing is smooth minute surface, and it is residual to remove polishing fluid with deionized water rinsing.
(5) be anode with the encapsulation aluminium flake, the plastic packaging cover is windowed side over against the negative electrode platinized platinum, carries out an anodic oxidation.Electrolytic solution is 0.4mol/L oxalic acid (analytical pure, massfraction is greater than 99.5%) solution, and solution temperature is controlled to be 4～6 ℃, and voltage constant is 45V, oxidization time 2 hours.In the whole electrolytic process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts.After oxidation was accomplished, it was residual to remove electrolytic solution with deionized water rinsing.
(6) go the once oxidation film to adopt phosphoric acid (analytical pure; Massfraction is greater than 85.0%) and chromic acid (analytical pure chromium trioxide; Massfraction is greater than 99.0%) mixing solutions (wherein phosphoric acid concentration is 6wt%, and chromic acid concentration is 1.8wt%) immersion, 60 ℃ of mixing solutions temperature; Soak time 2 hours, and magnetic agitation.Whole going in the once oxidation membrane process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts.After soaking end, it is residual to remove solution with deionized water rinsing.
(7) the same step of condition (5) is carried out two-step anodization to the aluminium flake exposure, and oxidization time is 4 hours.In the whole electrolytic process, plastic packaging gum cover good seal.After oxidation was accomplished, it was residual to remove electrolytic solution with deionized water rinsing.
(8) the plastic packaging gum cover is cut off removal, this moment, aluminium flake simultaneously was the pellumina that behind secondary oxidation, forms, and another side is that unreacted is aluminium base; Be equipped with a same big or small plastic packaging gum cover in addition, a side is opened onesize window, this time with aluminium flake oxidation face package isolation, and aluminium base exposure of unreacted; Aluminium flake behind the plastic packaging is placed saturated cupric chloride (analytical pure, the Copper dichloride dihydrate massfraction is greater than 99.0%) solution, expose aluminium base will being removed, the window that a side exposes becomes transparent at this moment; In the whole aluminium flake reaction process, plastic packaging gum cover good seal; After reaction was accomplished, it was residual to remove solution with deionized water rinsing.
(9) the plastic packaging aluminium flake was placed in 5wt% phosphoric acid (analytical pure, massfraction is greater than the 85.0%) solution 80 minutes, remove the alumina formwork blocking layer, finally obtain the bilateral alumina formwork.In this process, plastic packaging gum cover good seal.
(10) the plastic packaging gum cover is cut off removal, get an amount of template and do the discovery of SEM morphology analysis: the pore size of template distribution range is narrower, is about 60nm; The duct degree of order is higher, is arranged in parallel; Thickness is about 40 μ m.Because the garment bag protection is nearly all arranged in the whole process of preparation, and it is high to obtain success ratio complete, no damaged alumina formwork.
Embodiment 3
(1) with high-purity aluminium flake (purity 99.999%; Beijing Non-ferrous Metal and Rare-earth Application Inst.) be cut into the square of 70 * 50mm, ultrasonic (ultrasonic frequency 40kHz) cleaned 5 minutes in acetone (analytical pure, massfraction is greater than 99.5%); Behind deionized water rinsing; Ultrasonic (ultrasonic frequency 40kHz) cleaned 15 minutes in absolute ethyl alcohol (analytical pure, massfraction is greater than 99.7%), and be air-dry.
(2) aluminium flake is placed box High Temperature Furnaces Heating Apparatus (KSL-1100X, brilliant Materials Technology Ltd. of Hefei section) annealing 5 hours, 500 ℃ of annealing temperatures.
(3) adopt the common rectangular plastic sealing of 95 * 75mm specification cover, and simultaneously cut out 60 * 40mm specification rectangle window at it; The aluminium flake of will annealing places plastic packaging gum cover plastic packaging sealing (F9061 type plastic packaging machine of one mind).
(4) with constant voltage mode the encapsulation aluminium flake is carried out electrochemical etching.Polishing fluid is 4: 1 absolute ethyl alcohol of volume ratio (analytical pure, massfraction is greater than 99.7%), perchloric acid (analytical pure, massfraction is greater than 70.0%) mixing solutions.Aluminium flake is an anode, and the plastic packaging gum cover is windowed side over against the negative electrode platinized platinum.Polishing voltage is chosen as 20V, 15 minutes time.Use magnetic stirring apparatus in the polishing process, make solution temperature and concentration even as far as possible.In the whole polishing process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts.Aluminium flake surface after the polishing is smooth minute surface, and it is residual to remove polishing fluid with deionized water rinsing.
(5) be anode with the encapsulation aluminium flake, the plastic packaging cover is windowed side over against the negative electrode platinized platinum, carries out an anodic oxidation.Electrolytic solution is 0.4mol/L oxalic acid (analytical pure, massfraction is greater than 99.5%) solution, and solution temperature is controlled to be 4～6 ℃, and voltage constant is 45V, oxidization time 2 hours.In the whole electrolytic process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts.After oxidation was accomplished, it was residual to remove electrolytic solution with deionized water rinsing.
(6) go the once oxidation film to adopt phosphoric acid (analytical pure; Massfraction is greater than 85.0%) and chromic acid (analytical pure chromium trioxide; Massfraction is greater than 99.0%) mixing solutions (wherein phosphoric acid concentration is 6wt%, and chromic acid concentration is 1.8wt%) immersion, 60 ℃ of mixing solutions temperature; Soak time 2 hours, and magnetic agitation.Whole going in the once oxidation membrane process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts.After soaking end, it is residual to remove solution with deionized water rinsing.
(7) the same step of condition (5) is carried out two-step anodization to the aluminium flake exposure, and oxidization time is 6 hours.In the whole electrolytic process, plastic packaging gum cover good seal.After oxidation was accomplished, it was residual to remove electrolytic solution with deionized water rinsing.
(8) the plastic packaging gum cover is cut off removal, this moment, aluminium flake simultaneously was the pellumina that behind secondary oxidation, forms, and another side is that unreacted is aluminium base; Be equipped with a same big or small plastic packaging gum cover in addition, a side is opened onesize window, this time with aluminium flake oxidation face package isolation, and aluminium base exposure of unreacted; Aluminium flake behind the plastic packaging is placed saturated cupric chloride (analytical pure, the Copper dichloride dihydrate massfraction is greater than 99.0%) solution, expose aluminium base will being removed, the window that a side exposes becomes transparent at this moment; In the whole aluminium flake reaction process, plastic packaging gum cover good seal; After reaction was accomplished, it was residual to remove solution with deionized water rinsing.
(9) the plastic packaging aluminium flake was placed in 5wt% phosphoric acid (analytical pure, massfraction is greater than the 85.0%) solution 80 minutes, remove the alumina formwork blocking layer, finally obtain the bilateral alumina formwork.In this process, plastic packaging gum cover good seal.
(10) the plastic packaging gum cover is cut off removal, get an amount of template and do the discovery of SEM morphology analysis: the pore size of template distribution range is narrower, is about 60nm; The duct degree of order is higher, is arranged in parallel; Thickness is about 60 μ m.Because the garment bag protection is nearly all arranged in the whole process of preparation, and it is high to obtain success ratio complete, no damaged alumina formwork.
Above embodiment proves that the different secondary oxidation time can obtain the alumina formwork of different thickness down, has proved that the plastic packaging technology can effectively be applied to the preparation of anodic oxidation aluminium formwork.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. method of utilizing plastic package process to prepare anodic oxidation aluminium formwork is characterized in that comprising following steps:
(1) in aluminium flake electrochemical etching process, utilize the face seal of plastic packaging to aluminium flake, another side exposes polishing;
(2) in the aluminium flake anode oxidation process,, only carry out anodic oxidation to exposing polished surface because plastic packaging is isolated;
(3) in going aluminium base process, utilize plastic packaging to the alumina formwork seal protection, aluminium base face is exposed in the solution and is removed, and obtains anodic oxidation aluminium formwork.
2. the method for utilizing plastic package process to prepare anodic oxidation aluminium formwork according to claim 1 is characterized in that comprising following steps:
(1) cleaning aluminium flake to its surperficial greasy dirt removes;
(2) with cleaned annealing aluminum sheet;
(3) aluminium flake of will annealing places the plastic packaging gum cover plastic packaging sealing that a side windows, and the one side that is sealed is not for reacting or handle;
(4) with constant voltage mode the encapsulation aluminium flake is carried out electrochemical etching; Polishing fluid is the absolute ethyl alcohol/perchloric acid mixing solutions of 4: 1 by volume proportionings; Aluminium flake is an anode, and the plastic packaging gum cover is windowed side over against the negative electrode platinized platinum; Polishing voltage 15～20V, 10～15 minutes time; Use magnetic stirring apparatus in the polishing process; In the whole polishing process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts; Aluminium flake surface after the polishing is smooth minute surface, and it is residual to remove polishing fluid with washed with de-ionized water;
(5) be anode with the encapsulation aluminium flake, the plastic packaging cover is windowed side over against the negative electrode platinized platinum, carries out an anodic oxidation; Electrolytic solution is the 0.4mol/L oxalic acid solution, and the oxalic acid solution temperature is 4～6 ℃, and voltage constant is 40～50V, and oxidization time is 2～4 hours; In the whole anode oxidation process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts; After oxidation was accomplished, it was residual to remove electrolytic solution with washed with de-ionized water;
(6) remove the once oxidation film: adopt the mixing solutions of phosphoric acid and chromic acid to soak, wherein phosphoric acid concentration is 6wt%, and chromic acid concentration is 1.8wt%; The mixing solutions temperature of phosphoric acid and chromic acid is 60～65 ℃, soaked 2～4 hours, and magnetic agitation; Whole going in the once oxidation membrane process, plastic packaging gum cover good seal, only the aluminium flake exposure reacts; After soaking end, it is residual to remove solution with washed with de-ionized water;
(7) the same step of condition (5) is carried out two-step anodization to the aluminium flake exposure, and oxidization time is 2～6 hours; In the whole electrolytic process, plastic packaging gum cover good seal; After oxidation was accomplished, it was residual to remove electrolytic solution with washed with de-ionized water;
(8) the plastic packaging gum cover is cut off removal, this moment, aluminium flake simultaneously was the pellumina that behind secondary oxidation, forms, and another side is that unreacted is aluminium base; Be equipped with a same big or small plastic packaging gum cover in addition, a side is opened onesize window, this time with aluminium flake oxidation face package isolation, and aluminium base exposure of unreacted; Aluminium flake behind the plastic packaging is placed saturated Cupric Chloride Solution, expose aluminium base will being removed, the window that a side exposes becomes transparent at this moment; In the whole aluminium flake reaction process, plastic packaging gum cover good seal; After reaction was accomplished, it was residual to remove solution with washed with de-ionized water;
(9) the plastic packaging aluminium flake being placed concentration is that the phosphoric acid solution of 5wt% soaked 40～80 minutes, to remove the alumina formwork blocking layer, must arrive the aperture and be about the bilateral alumina formwork that 60nm, thickness are about 20～60 μ m.
3. the method for utilizing plastic package process to prepare anodic oxidation aluminium formwork according to claim 2; It is characterized in that: the cleaning described in the step (1) is for to carry out through following steps: ultrasonic cleaning is 5 minutes in acetone; Behind deionized water rinsing; Ultrasonic cleaning is 15 minutes in absolute ethyl alcohol, and is air-dry.
4. the method for utilizing plastic package process to prepare anodic oxidation aluminium formwork according to claim 3 is characterized in that: described ultransonic frequency is 40kHz.
5. the method for utilizing plastic package process to prepare anodic oxidation aluminium formwork according to claim 2 is characterized in that: the annealed condition described in the step (2) is 400～500 ℃ of annealing 3～5 hours.
6. an anodic oxidation aluminium formwork prepares through each described method of claim 1～5.
7. each described method application in the high-quality anodic oxidation aluminium formwork of mass preparation that utilizes plastic package process to prepare anodic oxidation aluminium formwork of claim 1～5.
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| CN104278308A (en) * | 2013-07-10 | 2015-01-14 | 中国科学院大连化学物理研究所 | Preparation method of though hole anode aluminum oxide |
| CN104630874A (en) * | 2015-01-20 | 2015-05-20 | 北方工业大学 | Method for completely separating film from film composite material |
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| CN107164795B (en) * | 2017-05-09 | 2019-02-15 | 电子科技大学 | A kind of bilateral AAO template and its preparation method and application |
| CN110993864A (en) * | 2019-11-21 | 2020-04-10 | 四川新敏雅电池科技有限公司 | Battery separator, method for manufacturing same, and lithium ion battery |
| CN111962127A (en) * | 2020-07-31 | 2020-11-20 | 常州费曼生物科技有限公司 | Single-side sealing method of anodic aluminum oxide porous membrane |
| CN112277406A (en) * | 2020-10-29 | 2021-01-29 | 河南省科学院应用物理研究所有限公司 | High-reliability aluminum-based copper-clad plate and preparation method thereof |
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