CN102839408B - The method of oversized hole spacing multiaperture pellumina is prepared in ultrasonic wave added anodic oxidation - Google Patents
The method of oversized hole spacing multiaperture pellumina is prepared in ultrasonic wave added anodic oxidation Download PDFInfo
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Abstract
The present invention relates to porous anodic alumina films, refer in particular to the method that oversized hole spacing multiaperture pellumina is prepared in ultrasonic wave added anodic oxidation.The present invention is used in citric acid electrolytic solution and adds ethanol raising electrolysis voltage, improves electrolysis speed, realize extra-high pressure (& gt in conjunction with ultrasonic technique; 500V) stablize electrolysis, and obtain the oversized hole spacing PAA of pitch of holes more than 1 micron.The present invention only needs two-step anodization technique, does not have rigors to aluminium flake pre-treatment, does not need complicated annealing, the pre-treatment step such as polishing or prepatterned; The present invention does not need to need extremely low temperature as hard anodizing in electrolytic process, and in very wide temperature range, (0-30 degree Celsius) can both carry out stable growth.
Description
Technical field
The present invention relates to porous anodic alumina films, refer in particular to the method that oversized hole spacing multiaperture pellumina is prepared in ultrasonic wave added anodic oxidation, belong to metal surface treatment technology and nanosecond science and technology field, its Application Areas includes non-ferrous metal surface treatment and nanostructure fabrication of new materials and application.
Background technology
Porous anodic aluminium oxide, PorousAnodicAlumina, PAA, not only extremely important to aluminum metal surface treatment, be also the important template of nano structural material preparation and assembling simultaneously; PAA typical structure is circular port periodic arrangement, and form nano-pore array structure, the hole wall between Kong Yukong is made up of amorphous nickel/phosphorus/aluminium oxide; The pore size of PAA is a very important parameter, such as determining the size retaining object during filtering membrane, the yardstick of prepared nano material is determined, the pore size of the PAA that anodic oxidation obtains and electrolysis voltage, the parameter correlations such as temperature and time when using as template.The aperture of PAA is by the further reaming of phosphoric acid, until hole wall is 10 ran; As, in 0.3M oxalic acid, electrolysis voltage is 40V, and electrolysis temperature is 0-5
ounder C, the PAA template initial aperture that anodic oxidation obtains is 40nm, and initial apertures spacing is 100nm, by controlling phosphoric acid reaming procedure, aperture can from 40nm to 90nm consecutive variations, pitch of holes is constant, therefore, the pitch of holes of PAA determines the adjustable extent in PAA aperture.
The pitch of holes of PAA is mainly determined by electrolysis voltage, and substantially presents linear proportional relation with electrolysis voltage, and the pitch of holes that therefore will improve PAA mainly will improve electrolysis voltage; In 3wt% phosphoric acid solution, under electrolysis voltage can bring up to 195V, in 1vol% phosphoric acid solution, 273K, electrolysis voltage can bring up to 235V, obtains the PAA film of 480nm pitch of holes; In the solution of 4wt% oxysuccinic acid, electrolysis voltage is 220V, and the pitch of holes of acquisition is about the PAA film of 550nm; The PAA film that average pitch of holes is about 600nm is obtained under 240V, 274K in 2wt% tartaric acid solution.In citric acid electrolytic solution, electrolysis voltage can reach 240V.
Great many of experiments shows, although electrolysis voltage can be risen to more than 200V in the weak acid such as citric acid and oxysuccinic acid, rise to the even higher very difficulty of 300V, and growth velocity is very low; 40V electrolysis voltage in 0.3M oxalic acid, the growth velocity of 0-5 degree Celsius, PAA is 3-5 μm/h, but corresponding growth velocity only has 1-2 μm/h in the electrolytic solution such as citric acid and oxysuccinic acid; Add ethanol in the electrolytic solution, ethylene glycol, or polyoxyethylene glycol, electrolysis voltage can be improved further, but relative to not adding organic electrolytic solution, the growth velocity of PAA is lower; Therefore, need to seek a kind ofly to stablize electrolysis under extra-high pressure and the moderate PAA preparation technology of growth velocity, widen the pitch of holes size of PAA further.
Summary of the invention
(current electrolysis under voltage is to prepare the PAA that aperture can get at micron to the present invention is directed to many deficiencies of the oversized hole spacing PAA technique set forth in technical background, and the growth velocity of PAA is lower etc.), be used in citric acid electrolytic solution and add ethanol raising electrolysis voltage, electrolysis speed is improved in conjunction with ultrasonic technique, and realize extra-high pressure (>500V) and stablize electrolysis, and obtain the oversized hole spacing PAA of pitch of holes more than 1 micron; The present invention only needs two-step anodization technique, does not have rigors to aluminium flake pre-treatment, does not need complicated annealing, the pre-treatment step such as polishing or prepatterned; The present invention does not need to need extremely low temperature as hard anodizing (HardAnodization) in electrolytic process, and in very wide temperature range, (0-30 DEG C) can both carry out stable growth.
To achieve these goals, the present invention is achieved through the following technical solutions the preparation of oversized hole spacing PAA: the first step, take aluminium flake as anode, the mixed electrolytic solution of configuration citric acid solution and dehydrated alcohol, electrolytic solution is made to be in ultrasonic state, electrolysis time 0.5-2 hour; Second step: remove PAA film in the mixing solutions of phosphoric acid and chromic acid; 3rd step: electrolyte system, electrolysis voltage are identical with the first step with temperature, electrolysis time hole depth is as required determined.
The described the first step, aluminium flake specifically refers to that purity is higher than 99%, and thickness is the aluminium flake of 0.05-1mm, through acetone and washed with de-ionized water post-drying as anode, with graphite, stereotype or platinum for negative electrode; The volume ratio of citric acid and dehydrated alcohol is 1:1 ~ 2, and the concentration of citric acid is 0.3M, and ultrasonic power and frequency are respectively 100-200W and 35 ~ 50kHz, and electrolysis voltage is 500-750V, and electrolysis temperature is 0-30
oc, electrolysis time is 0.5-2h.
Described second step, in phosphoric acid and chromic acid mixing solutions, the weight percent of phosphoric acid is 6.0%, and the weight percent of chromic acid is 1.8%, and temperature is 60
oc, soaks the twice for the first step electrolysis time, i.e. 1-4h.
The 3rd described step, electrolysis voltage is identical with the first step, and electrolysis time determines the thickness of PAA film, and typical electrolysis time is 5 minutes to 2 hours.
Prepare the method for oversized hole spacing anodic alumina films by above-mentioned ultrasonic wave added, the oversized hole spacing of preparation is 1-1.5 μm.
Prepare the method for oversized hole spacing anodic alumina films by above-mentioned ultrasonic wave added, growth velocity reaches 4-60 μm/h.
The method of oversized hole spacing anodic alumina films is prepared by above-mentioned ultrasonic wave added, first time and for the second time electrolytic process stability are higher, no sample burns (electric field concentrates the Burning phenomenon caused), and PAA growth velocity slightly increases along with the raising of electrolyte temperature.
Prepare the method for oversized hole spacing anodic alumina films by above-mentioned ultrasonic wave added, the growth velocity of PAA film increases along with the raising of electrolysis voltage.
Prepare the method for oversized hole spacing anodic alumina films by above-mentioned ultrasonic wave added, the PAA film thickness of preparation increases along with electrolysis time and increases.
Ultrasonic wave added of the present invention prepares the method for oversized hole spacing anodic alumina films, and the growth velocity of PAA film is relevant with ultrasonic power, and ultrasonic power increases, and PAA layer-growth rate has increased slightly.
As shown from the above technical solution, ultrasonic wave added of the present invention prepares the method for oversized hole spacing anodic alumina films, and the advantage had compared with existing general technology has: 1, electrolysis voltage rises to 500-750V; 2, pitch of holes is 1-1.5 μm; 3, stable electrolysis process and wider temperature window; 4, the pre-treating technology such as high temperature annealing and chemical rightenning of aluminium is avoided; Therefore, the method that ultrasonic wave added described in the invention prepares oversized hole spacing anodic alumina films is a kind of simple, efficient and PAA preparation method with using value of easy care, the pore diameter range of PAA can be expanded to 1000-1500nm, realize the combination of nanometer-size and micro-meter scale aperture nanostructure, and the PAA film of micron-nanometer composite structure can be used in, and be applied to the preparation of micro-nanometer structural material further.
Accompanying drawing explanation
Fig. 1 is the cross-sectional scans Electronic Speculum figure of embodiment 1 sample;
Fig. 2 is the surface scan Electronic Speculum figure of embodiment 1 sample;
Fig. 3 is the surface scan Electronic Speculum figure after the reaming of embodiment 1 sample;
Fig. 4 is the cross-sectional scans Electronic Speculum figure of embodiment 2 sample;
Fig. 5 is the cross-sectional scans Electronic Speculum figure of embodiment 3 sample;
Fig. 6 is the cross-sectional scans Electronic Speculum figure of embodiment 4 sample;
Fig. 7 is the surface scan Electronic Speculum figure of embodiment 4 sample.
Embodiment
Content of the present invention is further illustrated below in conjunction with example:
case one:
The first step, by purity 99.999% thickness 100 μm of area 4cm
2high-purity aluminum foil, in acetone soak 2 minutes, acetone rinsing, deionized water rinsing post-drying, puts into electrolyzer as anode; Graphite Electrodes, area is 200cm
2.It is the citric acid of 0.3M and the ethanol of 2L that electrolytic solution consists of 1L concentration, and electrolyte temperature uses circulating refrigerator to be stabilized in 0-5
oc, electrolysis voltage 750V, ultrasonic power 100W, frequency 35kHz, electrolysis time 30 minutes.
Second step, soaks 1 hour in chromic acid.
3rd step, electrolysis 10 minutes under the processing condition identical with step one.
As shown in Figure 1, surface as shown in Figure 2 for the cross section structure of gained sample; From cross section, each hole is positioned at the mid-way of U-shaped unit.Hole between centers is 1.5 microns, electrolysis voltage-pitch of holes relation that 100nm pitch of holes keeps identical is obtained with electrolysis under 0.3M oxalic acid 40V, hole depth 1.5 microns, growth velocity reaches 9 μm/h, higher than general PAA growth velocity (0.3M oxalic acid 40V, typical growth rate is 3-5 μm/h); With general PAA unlike, the oversized hole spacing PAA hole inwall that the present invention obtains Non-smooth surface or vertically, this shows as the hole shape looks of not too rule in surperficial Photomicrograph, but for the duct utilizing PAA, the imperfect use not affecting duct on surface, on the contrary, when material is filled in such PAA duct, rough duct contributes to obtaining different structure.
Obtained sample is put into 5wt% phosphoric acid, 30 degrees Celsius, soak 10 hours, as shown in Figure 3, the aperture of PAA greatly increases surface topography, and pitch of holes does not change, and this result shows that the PAA aperture that the present invention obtains can reach more than 1 micron.
case row two:
The first step, by purity 99.999% thickness 100 μm of area 4cm
2high-purity aluminum foil, in acetone soak 2 minutes, acetone rinsing, deionized water rinsing post-drying, puts into electrolyzer as anode.Graphite Electrodes, area is 200cm
2.Electrolytic solution consists of 0.3M citric acid 1L and 1.5L ethanol, and electrolyte temperature uses circulating refrigerator to be stabilized in 15
oc, electrolysis voltage 600V, ultrasonic power 150W, frequency 50kHz, electrolysis time 30 minutes.
Second step, soaks 1 hour in chromic acid.
3rd step, electrolysis 20 minutes under the processing condition identical with step one.
The cross section structure of gained sample as shown in Figure 4.Hole between centers is about 1.2 μm, electrolysis voltage-pitch of holes relation that 100nm pitch of holes keeps identical is obtained with electrolysis under 0.3M oxalic acid 40V, hole depth about 7 μm, growth velocity reaches 21 μm/h, far above general PAA growth velocity (0.3M oxalic acid 40V, typical growth rate is 3-5 μm/h), and general PAA unlike, duct and non-fully be parallel to each other.
case row three:
The first step, by purity 99.999% thickness 100 μm of area 4cm
2high-purity aluminum foil, in acetone soak 2 minutes, acetone rinsing, deionized water rinsing post-drying, puts into electrolyzer as anode, Graphite Electrodes, and area is 200cm
2.Electrolytic solution consists of 0.3M citric acid 1L and 1L ethanol.Electrolyte temperature uses circulating refrigerator to be stabilized in 30
oc, electrolysis voltage 500V, ultrasonic power 200W, frequency 45kHz, electrolysis time 60 minutes.
Second step, soaks 2 hours in chromic acid.
3rd step, electrolysis 30 minutes under the processing condition identical with step one.
The cross section structure of gained sample as shown in Figure 5, hole between centers is about 1 μm, electrolysis voltage-pitch of holes relation that 100nm pitch of holes keeps identical is obtained with electrolysis under 0.3M oxalic acid 40V, hole depth about 12 μm, growth velocity reaches 24 μm/h, far above general PAA growth velocity (0.3M oxalic acid 40V, typical growth rate is 3-5 μm/h), with general PAA unlike, duct and non-fully be parallel to each other, and hole wall rough or vertical.
comparative example four:contrast with case one
The first step, by purity 99.999% thickness 100 μm of area 4cm
2high-purity aluminum foil, in acetone soak 2 minutes, acetone rinsing, deionized water rinsing post-drying, puts into electrolyzer as anode, Graphite Electrodes, and area is 200cm
2.Electrolytic solution consists of 0.3M citric acid 1L and 2L ethanol, and electrolyte temperature uses circulating refrigerator to be stabilized in 0-5
oc, electrolysis voltage 750V, do not have ultrasonic, electrolysis time 30min.
Second step, soaks 1h in chromic acid.
3rd step, electrolysis 10min under the processing condition identical with step one.
The surface of gained sample and cross section are as shown in Figures 6 and 7, distribute not specification and the very low pore structure of fraction of coverage can be seen from surperficial Photomicrograph, from cross section, any pore structure is almost can't see in each hole, form zone of oxidation thickness also only about 200nm, as shown in black arrow in Fig. 6, well below μm hole depth of 1.5 in case one.These results are compared with case one, show ultrasonicly to play vital effect in the present invention, if do not have ultrasonicly just cannot obtain good PAA pore passage structure in electrolytic process, and zone of oxidation synthesis speed is very low.
comparative example five: contrast with case two
The first step, by purity 99.999% thickness 100 μm of area 4cm
2high-purity aluminum foil, in acetone soak 2 minutes, acetone rinsing, deionized water rinsing post-drying, puts into electrolyzer as anode, Graphite Electrodes, and area is 200cm
2.Electrolytic solution consists of 0.3M citric acid 1L and 1.5L ethanol, and electrolyte temperature uses circulating refrigerator to be stabilized in 15
oc, electrolysis voltage 600V, ultrasonic power 300W, frequency 20kHz, electrolysis time 30min.
Second step, soaks 1h in chromic acid.
3rd step, electrolysis 20min under the processing condition identical with step one.
The surface of gained sample and cross section are similar to shown in Fig. 6 and 7 of comparative example 4, these results are compared with case 2, ultrasonic power and the selection of frequency play vital effect in the present invention, in electrolytic process, the selection of ultrasonic power and frequency just cannot not obtain good PAA pore passage structure in scope of the present invention, and zone of oxidation synthesis speed is very low.
Claims (5)
1. the method for oversized hole spacing multiaperture pellumina is prepared in ultrasonic wave added anodic oxidation, it is characterized in that comprising the steps: that (1) take aluminium flake as anode, described aluminium flake does not have rigors to pre-treatment, do not need complicated annealing, polishing or prepatterned pre-treatment step, the mixed electrolytic solution of configuration citric acid solution and dehydrated alcohol, makes electrolytic solution be in ultrasonic state, electrolysis time 0.5-2 hour; (2) in the mixing solutions of phosphoric acid and chromic acid, PAA film is removed; (3) electrolyte system, electrolysis voltage are identical with the first step with temperature, and electrolysis time hole depth is as required determined; The volume ratio of citric acid and dehydrated alcohol is 1:1 ~ 2, and the concentration of citric acid is 0.3M, and ultrasonic power and frequency are respectively 100-200W and 35 ~ 50kHz; Described oversized hole spacing is 1-1.5 μm.
2. the method for oversized hole spacing multiaperture pellumina is prepared in ultrasonic wave added anodic oxidation as claimed in claim 1, it is characterized in that: described step (1), aluminium flake specifically refers to that purity is higher than 99%, thickness is the aluminium flake of 0.05-1mm, and through acetone and washed with de-ionized water, with graphite, stereotype or platinum for negative electrode; Electrolysis voltage is 500-750V, and electrolysis temperature is 0-30
oc, electrolysis time is 0.5-2h.
3. the method for oversized hole spacing multiaperture pellumina is prepared in ultrasonic wave added anodic oxidation as claimed in claim 1, it is characterized in that: described step (2), in phosphoric acid and chromic acid mixing solutions, the weight percent of phosphoric acid is 6.0%, the weight percent of chromic acid is 1.8%, and temperature is 60
oc, soak time is the twice of the first step electrolysis time, i.e. 1-4h.
4. the method for oversized hole spacing multiaperture pellumina is prepared in ultrasonic wave added anodic oxidation as claimed in claim 1, and it is characterized in that: described step (3), electrolysis time is 5 minutes to 2 hours.
5. the method for oversized hole spacing multiaperture pellumina is prepared in ultrasonic wave added anodic oxidation as claimed in claim 1, it is characterized in that: growth velocity reaches 4-60 μm/h.
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| CN103147108B (en) * | 2013-03-14 | 2016-03-16 | 山西师范大学 | A kind of anodic alumina films and preparation method thereof |
| CN106544712B (en) * | 2016-10-19 | 2019-06-07 | 陕西师范大学 | A kind of preparation method of orderly super large pitch of holes pellumina |
| CN106670744B (en) * | 2016-12-21 | 2018-09-25 | 西安理工大学 | A kind of preparation method of the wear-resisting hydrophobic sliding functional membrane of inner surface of bearing bush |
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| CN101139730A (en) * | 2007-06-12 | 2008-03-12 | 太原理工大学 | Strong anodic oxidation method for preparing porous pellumina |
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| WO2012054045A1 (en) * | 2010-10-21 | 2012-04-26 | Hewlett-Packard Development Company, L.P. | Method of forming a nano-structure |
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| US4481084A (en) * | 1984-04-16 | 1984-11-06 | Sprague Electric Company | Anodization of aluminum electrolyte capacitor foil |
| CN101139730A (en) * | 2007-06-12 | 2008-03-12 | 太原理工大学 | Strong anodic oxidation method for preparing porous pellumina |
| CN101603192A (en) * | 2009-07-14 | 2009-12-16 | 桂林理工大学 | A kind of method of utilizing commercial-purity aluminium to prepare porous anodic alumina films |
| WO2012054045A1 (en) * | 2010-10-21 | 2012-04-26 | Hewlett-Packard Development Company, L.P. | Method of forming a nano-structure |
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