CN100361240C - Nano holing method on surface of low-voltage anode foil for aluminium electrolytic capacitor - Google Patents
Nano holing method on surface of low-voltage anode foil for aluminium electrolytic capacitor Download PDFInfo
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- CN100361240C CN100361240C CNB2004100643407A CN200410064340A CN100361240C CN 100361240 C CN100361240 C CN 100361240C CN B2004100643407 A CNB2004100643407 A CN B2004100643407A CN 200410064340 A CN200410064340 A CN 200410064340A CN 100361240 C CN100361240 C CN 100361240C
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 27
- 239000011888 foil Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000003990 capacitor Substances 0.000 title claims abstract description 14
- 239000004411 aluminium Substances 0.000 title description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 32
- 230000003647 oxidation Effects 0.000 claims abstract description 28
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 23
- 238000005498 polishing Methods 0.000 claims abstract description 14
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims abstract description 9
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 239000005030 aluminium foil Substances 0.000 claims description 42
- 239000012528 membrane Substances 0.000 claims description 24
- 239000012530 fluid Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 5
- 238000002048 anodisation reaction Methods 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract 1
- 239000001117 sulphuric acid Substances 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 1
- 239000004744 fabric Substances 0.000 description 18
- 230000007797 corrosion Effects 0.000 description 12
- 238000005260 corrosion Methods 0.000 description 12
- 239000011148 porous material Substances 0.000 description 9
- 230000000903 blocking effect Effects 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- -1 chloro ion Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000001550 time effect Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Abstract
The present invention relates to a nanometer holing method for the surface of low-voltage anode foil for an aluminum electrolytic capacitor, which is a holing method for the surface of foil, particularly a nanometer holing method for the surface of low-voltage anode foil for an aluminum electrolytic capacitor. Surface cleaning and electrochemical polishing are carried out to aluminum foil, and the composition of a polishing solution comprises 80 to 160 of phosphoric acid, 0.1 to 1 of sulphuric acid and 50 to 100 of glycerol; the polished aluminum foil is put in the phosphoric acid solution for carrying out first anodic oxidation under the voltage of 20 to 120V, and then first film removal is carried out to a mixed solution of the phosphoric acid and a chromic acid until the surface of the mixed solution exposes an aluminum matrix; second oxidation and second film removal are carried out under the same experiment conditions as the first oxidation. The density and the hole diameter of a holed hole can be adjusted by adjusting a technical parameter, wherein the size of the hole diameter can be changed between 50 to 300 nm so as to be suitable for low-voltage foil in different application ranges. The method can realize high-density nanometer holing for the surface of low-voltage anode aluminum foil and can largely enhance the volume ratio capacitance of the low-voltage anode aluminum foil.
Description
Technical field
The present invention relates to a kind of paper tinsel surface bore distribution method, especially a kind of method that is used for the low-voltage anode foil nano surface cloth hole of aluminium electrolytic capacitor.
Background technology
Since German in 1938 produces in the world first high-purity aluminum foil electrolytic capacitor, because its capacitance per unit volume amount is big, oxide-film has advantages such as self-healing feature, low price, aluminium electrolytic capacitor becomes one of most popular electronic devices and components gradually.Development of science and technology has proposed more and more higher requirement to the miniaturization of electronic product, because the volume of the capacitance of capacitor and capacitor is closely related, thereby capacitor becomes the greatest factor of restriction miniaturization of electronic products.Improve the ratio electric capacity of aluminium electrolytic capacitor with aluminium foil, dwindling the aluminium electrolytic capacitor volume is a key technology that solves the miniaturization of electronic products problem.
In order to improve the ratio electric capacity of aluminium electrolytic capacitor, the effective surface area that adopts electrochemical corrosion to increase aluminium foil is present international technology, wherein mainly comprises the initiation (cloth hole) of the initial pit of aluminium foil surface and expansion (reaming) technology of aluminium foil pit.Aluminium foil generally can be divided into mesohigh paper tinsel, low blocking and Cathode Foil by purposes, and its manufacturing process differs widely.For low blocking, its manufacturing process mainly comprises aluminium foil surface cloth hole and two important steps of corrosion reaming, wherein aluminium foil surface cloth hole is vital for the ratio electric capacity that improves aluminium foil, have only pit at first suitable, that be evenly distributed, just may cooperate certain chambering process to obtain high specific volume, high-quality aluminium etched foil at the aluminium foil surface preparation scale.Main flow technology is to adopt the very high hard attitude aluminium foil of purity at present, through acid solution or alkali lye surface clean, behind the cloth hole, chloro ion-containing solution surface, through low-frequency ac galvano-cautery reaming, carries out the direct current anodization then in changing into liquid in the acid solution of chloride ion-containing.No matter the surface corrosion hole that obtains thus is uniformity, the hole density that distributes, or hole size all is difficult to control, relies on the quality and the surface appearance of aluminium foil raw material to a great extent.
For low blocking, no matter be corrosion cloth hole or corrosion reaming, at present traditional technology all exists and generates the hole technical problems such as uncertain, out-of-shape, the direction of growth be uncontrollable that distribute, thereby reduced the controllability of production technology, also made the ratio electric capacity of low blocking be significantly less than theoretical value.Though domestic and international research person has carried out a large amount of effort for many years, progress is not still not clearly.Another uncontrollable factor is the reset condition of aluminium foil raw material (light paper tinsel).All must influence the cloth hole and the corrosion process of aluminium foil as factors such as the manufacturing process of light paper tinsel, surface appearance, crystalline condition, dopant species, amount of impurities.This will seek survival product producer will be at the light paper tinsel of separate sources, formulate corresponding surperficial cloth hole and corrosion chambering process, thereby cause the poor for applicability of general technology, the electrolysis aluminium foil quality is dispersed big, and the formulation of special process also must make industrial cost greatly increase.
Summary of the invention
The object of the present invention is to provide and a kind ofly can be convenient to adjust the density in cloth hole and the size of hole, have the bore distribution method of the strong low-voltage anode foil of applicability and controllability according to different specification requirements.
Technical scheme provided by the invention comprises steps such as light paper tinsel surface clean, electropolishing, once oxidation, a membrane removal, secondary oxidation, secondary membrane removal.Concrete processing step is as follows:
1) cleaning and electropolishing: earlier the aluminium foil surface is carried out surface clean such as conventional oil removing, oxide film dissolving, then aluminium foil is placed 50～90 ℃ polishing fluid, apply 5～20V voltage and carry out electrochemical polish 1～30min, polishing fluid by volume consist of phosphoric acid: sulfuric acid: glycerine=(80～160): (0.1～1): (50～100).
2) once oxidation and membrane removal: polished aluminium foil is placed 1%～10% phosphoric acid solution, under 20～120V voltage, carry out an anodic oxidation, oxidization time 3～30min.The mixed solution of using 5%～30% (wt) phosphoric acid and 1%～12% (wt) chromic acid then is 30～80 ℃ of following membrane removal 2～10min times, expose aluminum substrate to the surface till.
3) secondary oxidation and membrane removal: use the experiment condition identical to carry out secondary oxidation and secondary membrane removal with once oxidation, soon the aluminium foil after once oxidation and the membrane removal places 1%～10% phosphoric acid solution once more, under 10～120V voltage, carry out two-step anodization, oxidization time 3～30min.The mixed solution of using 5%～30% (wt) phosphoric acid and 1%～12% (wt) chromic acid then is 30～80 ℃ of following membrane removal 2～10min times, expose aluminum substrate to the surface till.
Adjusting process controllable parameters control surface cloth hole hole density and aperture, when phosphoric acid concentration was high, the aperture was bigger, and hole wall is thinner, is easy between the Kong Yukong be communicated with.When phosphoric acid concentration was low, the hole growth was slower, needed to prolong the anodised time; The height of anodic oxidation voltage has determined the size in the aperture of final generation, and high voltage obtains wide-aperture hole, and low-voltage obtains the hole of small-bore, but after voltage acquired a certain degree, the aperture no longer increased; Anodised time effects pore size obtains wide-aperture hole for a long time, and the short time obtains little hole, aperture, but the time oversizely cause the aluminium foil excessive thinning easily, and influence the efficient of technology; Temperature also has certain influence to the formation of hole, and usually, if the temperature height, then hole density is big, and the aperture is little, and oxidation rate is fast.By regulating these parameters, can adjust cloth hole hole density and aperture, wherein pore size can change between 50～300nm, to be applicable to the low blocking of different application scope.
Description of drawings
Fig. 1 is the aluminium foil surface SEM photo behind the secondary oxidation.
Fig. 2 is the aluminium foil surface SEM photo after the secondary membrane removal.
Fig. 3 is the aluminium foil surface SEM photo after corrosion after a while.
Fig. 4 is for adopting the aluminium foil surface SEM photo in traditional handicraft cloth hole.
Fig. 5 is for adopting the aluminium foil surface SEM photo after traditional handicraft cloth hole and reaming are corroded.
Embodiment:
The invention will be further described below by embodiment.
Embodiment 1: surperficial grease is removed with acetone in the aluminium foil surface, remove oxide-film with NaOH, be placed on then in 70 ℃ the polishing fluid, apply 10V voltage and carry out the about 5min of electrochemical polish, polishing fluid consist of phosphoric acid: sulfuric acid: glycerine (v/v)=115: 0.5: 85; Adopt 3% (wt) H
3PO
4Be electrolyte, carry out anodic oxidation 15min one time under 60V voltage, expose aluminum substrate with the mixed solution of 15% (wt) phosphoric acid and 5% (wt) chromic acid on 60 ℃ of membrane removal to surfaces, carry out secondary oxidation and membrane removal then, condition is with for the first time identical.Fig. 1 is the SEM photo of aluminium foil surface behind the above-mentioned technology secondary oxidation of employing, and as can be seen, surface distributed the comparatively pit of homogeneous of size, and hole size is between 93～220nm, and average pore size is 152nm.
Embodiment 2: the aluminium foil surface is carried out surface clean such as conventional oil removing, oxide film dissolving by embodiment 1 method, be placed on then in 40 ℃ the polishing fluid, apply 6V voltage and carry out the about 25min of electrochemical polish, polishing fluid consist of phosphoric acid: sulfuric acid: glycerine=150: 0.7: 100.Adopt 10% (wt) H
3PO
4Be electrolyte, carry out anodic oxidation 30min one time under 30V voltage, expose aluminum substrate with the mixed solution of 6% (wt) phosphoric acid and 2% (wt) chromic acid on 80 ℃ of membrane removal to surfaces, carry out secondary oxidation and membrane removal then, condition is with for the first time identical.Obtain the comparatively pit of homogeneous of size at aluminium foil surface, average pore size is 78nm.
Embodiment 3: the aluminium foil surface is carried out surface clean such as conventional oil removing, oxide film dissolving, be placed on then in 70 ℃ the polishing fluid, applying 18V voltage carries out the about 3min of electrochemical polish, polishing fluid consist of phosphoric acid: sulfuric acid: glycerine=90: 0.3: 60.Adopt 8% (wt) H
3PO
4Be electrolyte, carry out anodic oxidation 15min one time under 80V voltage, expose aluminum substrate with the mixed solution of 27% (wt) phosphoric acid and 10% (wt) chromic acid on 40 ℃ of membrane removal to surfaces, carry out secondary oxidation and membrane removal then, condition is with for the first time identical.Obtain the comparatively pit (see figure 2) of homogeneous of size at aluminium foil surface, hole size is between 136～274nm, and average pore size is 220nm.Fine rule is an oxidation aluminum steel remaining after the membrane removal in Fig. 2.Line directly is 30～12nm, and length is 1 μ m.As can be seen from Figure 2, the membrane removal step can be removed alumina layer substantially effectively, the hole of aluminum substrate remained on surface and alumina layer basically identical.
Embodiment 4: the aluminium foil surface is carried out surface clean such as conventional oil removing, oxide film dissolving, be placed on then in 70 ℃ the polishing fluid, applying 10V voltage carries out the about 5min of electrochemical polish, and the composition of polishing fluid is identical with embodiment 1 with preparation.Adopt 1% (wt) H
3PO
4Be electrolyte, carry out anodic oxidation 15min one time under 110V voltage, 50 ℃ of membrane removals, carry out secondary oxidation and membrane removal with the mixed solution of 20% (wt) phosphoric acid and 7% (wt) chromic acid then, condition is with for the first time identical.Obtain the comparatively pit of homogeneous of size at aluminium foil surface, hole size is between 261～117nm, and average pore size is 230nm.Above-mentioned aluminium foil in 7% (wt) HCl, is applied 0.4A/cm
2Direct current, corrosion 3min, corrosion back aluminium foil surface SEM photo is seen Fig. 3.As can be seen from Figure 3, aluminium surface hole defect state does not have to change substantially before and after the corrosion, and the generation of corrosion hole is that the hole in cloth hole surfacewise carries out to the depths.Fig. 4 is for adopting the aluminium foil surface SEM photo in traditional handicraft cloth hole.As can be seen from Figure 4, adopt the cloth hole technology of traditional handicraft, the pore size distribution that obtains is inhomogeneous, and aperture difference is big.In addition, the vestige that striped is rolled on the aluminium foil surface still as seen, so the aluminium foil surface pattern to be rolled factor affecting such as striped bigger.
Fig. 5 is for adopting the aluminium foil surface SEM photo after also corrode in order traditional handicraft cloth hole.As can see from Figure 5, the corrosion hole that traditional handicraft obtains is the spongelike structure that macroscopic void comprises small holes, and etch pit distributes very inhomogeneous, so the unit-area capacitance value is inevitable not high.
Embodiment 5～11: by changing technological parameter, and control surface cloth hole hole density and aperture, table 1 has been listed its experiment parameter of selecting for use and the average pore size of the hole that finally obtains.
The different experiment parameter of table 1. control can obtain the aperture that different size distributes
| Embodiment | Glossing | Phosphoric acid concentration (%) | Film-removing technology | First step voltage (V) | The first step time (min) | The second step voltage (V) | Second time in step (min) | Average pore size (nm) |
| 05 | With embodiment 3 | 10 | With embodiment 1 | 40 | 20 | 40 | 20 | 75 |
| 06 | With embodiment 1 | 8 | With embodiment 3 | 50 | 10 | 50 | 10 | 90 |
| 07 | With |
8 | With embodiment 2 | 60 | 5 | 60 | 5 | 83 |
| 08 | With embodiment 1 | 3 | With embodiment 3 | 80 | 5 | 80 | 10 | 96 |
| 09 | With embodiment 2 | 4 | With |
80 | 5 | 80 | 15 | 124 |
| 10 | With embodiment 3 | 5 | With embodiment 2 | 90 | 10 | 90 | 10 | 193 |
| 11 | With embodiment 2 | 5 | With |
100 | 10 | 100 | 15 | 219 |
Claims (1)
1. the nano holing method on surface of low-voltage anodic foil for aluminum electrolytic capacitor is characterized in that its step is as follows:
1) cleaning and electropolishing: earlier conventional oil removing, oxide film dissolving surface clean are carried out in the aluminium foil surface, then aluminium foil is placed 50～90 ℃ polishing fluid, apply 5～20V voltage and carry out electrochemical polish 1～30min, polishing fluid by volume consist of phosphoric acid: sulfuric acid: glycerine=80～160: 0.1～1: 50～100;
2) once oxidation and membrane removal: polished aluminium foil is placed 1%～10% phosphoric acid solution, under 20～120V voltage, carry out an anodic oxidation, oxidization time 3～30min, the mixed solution of using 5%～30% (wt) phosphoric acid and 1%～12% (wt) chromic acid then is till 30～80 ℃ of following membrane removals are exposed aluminum substrate to the surface;
3) secondary oxidation and membrane removal: the aluminium foil after once oxidation and the membrane removal is placed 1%～10% phosphoric acid solution once more, under 20～120V voltage, carry out two-step anodization, oxidization time 3～30min, the mixed solution of using 5%～30% (wt) phosphoric acid and 1%～12% (wt) chromic acid then is till 30～80 ℃ of following membrane removals are exposed aluminum substrate to the surface.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100643407A CN100361240C (en) | 2004-08-20 | 2004-08-20 | Nano holing method on surface of low-voltage anode foil for aluminium electrolytic capacitor |
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| CNB2004100643407A CN100361240C (en) | 2004-08-20 | 2004-08-20 | Nano holing method on surface of low-voltage anode foil for aluminium electrolytic capacitor |
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| CN1598985A CN1598985A (en) | 2005-03-23 |
| CN100361240C true CN100361240C (en) | 2008-01-09 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100527300C (en) * | 2007-07-13 | 2009-08-12 | 厦门大学 | Method for modifying surface of aluminum electrode foil |
| CN103695983B (en) * | 2013-12-16 | 2016-05-04 | 陕西师范大学 | The preparation method of the controlled aluminium surface periodic nanometer hole texture of a kind of size |
| CN104611760B (en) * | 2014-12-15 | 2017-05-10 | 肇庆华锋电子铝箔股份有限公司 | Electronic aluminum foil energy conservation and environmental protection electrochemical corrosion expansion method |
| CN107254708B (en) * | 2017-06-23 | 2019-01-11 | 乳源县立东电子科技有限公司 | The method of two sections of cloth holes of low voltage anode aluminum foil |
| CN108648915A (en) * | 2018-05-09 | 2018-10-12 | 大连理工大学 | A kind of electrode aluminum foil preparation for high power capacity aluminium electrolutic capacitor |
| CN113089069B (en) * | 2020-01-09 | 2022-05-20 | 山西沃特海默新材料科技股份有限公司 | Preparation method of microporous foil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09516A (en) * | 1995-06-23 | 1997-01-07 | Toshiba Medical Eng Co Ltd | X-ray computer tomographic system |
| CN1391243A (en) * | 2002-07-24 | 2003-01-15 | 扬州宏远电子有限公司 | Process for preparing 35Vw and 50Vw anode foil with high specific capacity and low contact resistance |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09516A (en) * | 1995-06-23 | 1997-01-07 | Toshiba Medical Eng Co Ltd | X-ray computer tomographic system |
| CN1391243A (en) * | 2002-07-24 | 2003-01-15 | 扬州宏远电子有限公司 | Process for preparing 35Vw and 50Vw anode foil with high specific capacity and low contact resistance |
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Address after: 526060 Duanzhou Industrial City, Zhaoqing City, Guangdong Province Co-patentee after: Zhaoqing Gaoyao Huafeng Electronic aluminium foil Co., Ltd. Patentee after: Guangdong Huafeng New Energy Technology Co., Ltd. Address before: 526060 Duanzhou Industrial City, Zhaoqing City, Guangdong Province Co-patentee before: Zhaoqing Gaoyao Huafeng Electronic aluminium foil Co., Ltd. Patentee before: Zhaoqing Huafeng Electronic Aluminum Foil Co., Ltd. |