CN104505260A - Method for preparing mid-high voltage corrosion foil by using pulse DC superposed current - Google Patents
Method for preparing mid-high voltage corrosion foil by using pulse DC superposed current Download PDFInfo
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- CN104505260A CN104505260A CN201410728211.7A CN201410728211A CN104505260A CN 104505260 A CN104505260 A CN 104505260A CN 201410728211 A CN201410728211 A CN 201410728211A CN 104505260 A CN104505260 A CN 104505260A
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- 238000000034 method Methods 0.000 title claims abstract description 107
- 239000011888 foil Substances 0.000 title claims abstract description 47
- 230000007797 corrosion Effects 0.000 title abstract description 22
- 238000005260 corrosion Methods 0.000 title abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 79
- 239000000243 solution Substances 0.000 claims abstract description 27
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- -1 aluminum ions Chemical class 0.000 claims abstract description 5
- 239000005030 aluminium foil Substances 0.000 claims description 24
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 238000005868 electrolysis reaction Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000012958 reprocessing Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 4
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- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 3
- 238000006056 electrooxidation reaction Methods 0.000 description 3
- 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 description 3
- 238000006396 nitration reaction Methods 0.000 description 3
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- 239000004327 boric acid Substances 0.000 description 2
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- 238000010301 surface-oxidation reaction Methods 0.000 description 2
- HLLSOEKIMZEGFV-UHFFFAOYSA-N 4-(dibutylsulfamoyl)benzoic acid Chemical compound CCCCN(CCCC)S(=O)(=O)C1=CC=C(C(O)=O)C=C1 HLLSOEKIMZEGFV-UHFFFAOYSA-N 0.000 description 1
- 241000693079 Maloideae Species 0.000 description 1
- OTRAYOBSWCVTIN-UHFFFAOYSA-N OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N Chemical compound OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N OTRAYOBSWCVTIN-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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- 230000004913 activation Effects 0.000 description 1
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 125000005619 boric acid group Chemical group 0.000 description 1
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Abstract
The invention relates to a method for preparing a mid-high voltage corrosion foil by using pulse DC superposed current. The method comprises the following steps of first pretreatment, second pretreatment, first-stage hole generation, intermediate treatment, second-stage hole generation and after-treatment. According to the method, an oxidation film on the surface of an aluminum foil is removed by strongly alkaline solution via the first pretreatment, residual alkaline solution on the surface of the aluminum foil is neutralized by strongly acid solution via the second pretreatment, holes are generated by a pulse DC superposed current method via first-stage hole generation, radius and depth of the holes are further enlarged by direct current via intermediate treatment, and residual aluminum ions on the surface of the aluminum foil are chemically eroded by after-treatment via second-stage hole generation. The whole technical process is simple, adaptability to change of corrosion tank liquid is high and the generated corrosion holes are uniform and smooth so that electrostatic specific volume of the corrosion foil is greatly enhanced, mechanical property is excellent, and the limit that the hole generation process in the conventional corrosion technology cannot be performed in case of power outage is solved.
Description
Technical field
The present invention relates to the preparation field of mesohigh anodic attack paper tinsel, be specifically related to a kind of method that pulse direct current superimposed current prepares mesohigh etched foil.
Technical background
What traditional mesohigh anode foils adopted is chromic acid corrosion system, advantage is because the corrosive power of chromic acid itself is stronger, therefore required electric current is less, greater advantage is had in caloric value and static specific volume, but because chromic acid system faces more serious environmental protection pressure, abroad substantially stop using, in the middle of domestic enterprise is also actively eliminating.
Current main flow etching process both domestic and external is all generally mixed acid systems of sulfuric acid and hydrochloric acid, its typical process flow comprises pre-treatment → one-level hair engaging aperture → secondary chambering → reprocessing, the main purpose of pre-treatment is to dispel the greasy dirt on light paper tinsel surface, oxide-film and partial impurities, obtains light paper tinsel surface that is more even, activation; First process is the key of whole etching process, reasonably combined nitration mixture ratio, coordinate the key parameters such as electric current, electricity and temperature, thus formation is evenly distributed, the rational initial voids of density, because first process must continue to power up, therefore result in aluminium ion in hole can not get rid of in time, can not produce desirable tunnel model hole, hole produces fold, and some perforations growth turns to, produce branch hole, this just greatly reduces etched foil performance; Secondary chambering is then expand aperture and hole depth further, require different according to different operating voltage to corrosion hole, Secondary process uses the electrolysis tank of 2-5 V, general aperture requires larger, Secondary process electrolysis time is longer, because Secondary process generally adopts acid solution, can produce strong in corrosion phenomenon at long electrolytic process, therefore Secondary process generally can produce and comparatively serious degrade phenomenon, thus causes electrolysis institute subfam. Spiraeoideae to increase and the mechanical performance decline of aluminium foil; Last handling process is then clean aluminium residual in aluminium foil surface and hole, increases etched foil surface cleanness.
Summary of the invention
Summary of the invention
The object of the invention is to the defect and the deficiency that overcome prior art, a kind of method that pulse direct current superimposed current prepares the etched foil of mesohigh anode foils is proposed, the method can solve that one-level hair engaging aperture process Hole is uneven, caloric value is excessive and secondary chambering process degrade cause that weight-loss ratio is higher, mechanical performance and the problem such as electrostatic specific volume is on the low side.
In order to achieve the above object, technical scheme of the present invention provides a kind of preparation method of pulse direct current superimposed current mesohigh etched foil, comprises the following steps:
A) last process: sodium hydroxide solution light paper tinsel raw material being put into 0.5-1mol/L, at 30-40 DEG C of process 60-120Sec;
B) the first two process: the above-mentioned aluminium foil through last process being put into concentration is 1-5Wt% sulfuric acid and 10-20Wt% nitric acid mixed solution, at 55-70 DEG C of process 90-120Sec;
C) one-level hair engaging aperture: the aluminium foil after the first two process above-mentioned is put into sulfuric acid, the hydrochloric acid of 3-5Wt%, the aluminum ions tank liquor of 1-2Wt% that concentration is 30-50Wt%, electrolysis 50-80Sec at 60-80 DEG C;
D) process in: the aluminium foil through hair engaging aperture step process is put into 3-5%Wt% dilute phosphoric acid solution, at 55-65 DEG C of process 120-180Sec;
E) secondary hair engaging aperture: the aluminium foil processed in process is put into the calcium polystyreme sulphonate solution that tank liquor composition proportion is the nitric acid of 5-8Wt%, the aluminium ion of 0.2-0.5Wt% and 0.01-0.5Wt%, add electric treatment 12-18min at 65-80 DEG C of direct current;
F) reprocessing: put into by the aluminium foil through secondary hair engaging aperture containing 1-3Wt% nitric acid, the aluminum ions solution of 0.5-3Wt%, soaks 3-4min at 60-70 DEG C;
G) dry: the air dry oven that the aluminium foil through reprocessing puts into 80-120 DEG C is processed 2-5min, foil closing after drying.
Detailed Description Of The Invention
A kind of method preparing pulse direct current superimposed current mesohigh etched foil that technical scheme according to the present invention provides, because light paper tinsel surface oxidation film thickness and uniformity are directly connected to complexity and the uniformity of one-level hair engaging aperture process, therefore select suitable pre-treating technology extremely important.In the inventive solutions pre-treatment is divided into two steps, last process first carries out alkaline pretreated process to high-purity aluminum foil: working concentration is 0.5-1mol/L, be added with the phosphide element of 60-90ppm and the Ce elements sodium hydroxide solution of 20-40ppm, greasy dirt, dissolving partial surface oxidation film that 60-120Sec removes light paper tinsel surface is processed, acquisition surface uniform, the aluminium foil that oxide-film is thinner at the temperature of 30-40 DEG C; The first two process uses in acid solution and the process of light paper tinsel remained on surface alkaline matter: use 1-5Wt% sulfuric acid, 10-20Wt% nitric acid, the alkaline matter with light paper tinsel remained on surface in after 90-120Sec is processed under the temperature conditions of 55-70 DEG C, acidifying aluminium foil surface oxide-film, is conducive to before one-level hair engaging aperture, form equally distributed pitting point.
One-level hair engaging aperture is corroded: first process is the key of whole etching process, directly decide aperture density degree with whether even, traditional mesohigh etching process all adopts constant dc current chemical corrosion, its shortcoming is that the big current continued on the one hand can cause aluminium foil surface caloric value larger, thus easy etched foil outward appearance, there is deviation in the aspect such as capacity and buckling performance, the constant dc current continued on the other hand also can cause aluminium ion in corrosion process not discharge in time, the corrosion hole direction of growth is departed from even turn to, the inhomogeneities of corrosion hole longitudinal direction and useless hole of horizontal direction is caused to increase, thus reduce etched foil performance.Therefore, present invention employs the method for a kind of pulse direct current superimposed current corrosion, a single group or many group pulse, forward duty ratio 50-80%, Mean Forward Current is about 0.4-0.8A/cm
2the permanent direct current of the lasting 5-15A of applying one on the basis of forward time 100ms, namely ensureing the alternating corrosion realizing current on the basis of not power-off, thus meet small area analysis stage corrosion process aluminium foil surface dispel the heat in time and hole growth course aluminium ion exchanged in time.
Middle process: because the secondary chambering process general time is longer, in long acid soak, aluminium foil surface produces and degrades phenomenon, this significantly can reduce etched foil performance, therefore put in the middle of 3-5Wt% dilute phosphoric acid solution at middle treatment step, under the temperature conditions of 55-65 DEG C, process 120-180Sec, contribute to surface and form phosphate radical passivating film, thus in secondary chambering process, more electricity grows for the depth of hole, and while reducing energy consumption, less aluminium foil surface degrades.
According to the method preparing mesohigh etched foil that technique scheme provides, light paper tinsel raw material are through the process of high-temperature vacuum stepped annelaing, thickness is 110-130 μm, the high-purity aluminum foil of cubic texture >=92%.
According to the method preparing mesohigh etched foil that technique scheme provides, purity >=99.98% of light paper tinsel raw material, wherein the content of impurity element Pb, Zn, Mg, Cu, Fe and Si is respectively 0-1.0ppm, 2-3ppm, 3-7ppm, 40-70ppm, 5-15ppm, 5-25ppm.
According to the method preparing mesohigh etched foil that technique scheme provides, be added with phosphide element and Ce elements in the treatment fluid of last process, its content is respectively 60-90ppm and 20-40ppm.
According to the method preparing mesohigh etched foil that technique scheme provides, one-level hair engaging aperture apply the superimposed current that electric current is DC pulse.
According to the method preparing mesohigh etched foil that technique scheme provides, superimposed current increases a single group or many group pulse on the little galvanic basis of 10-20A, and wherein forward duty ratio is 50-80%, and Mean Forward Current is 0.4-0.8A/cm
2, the forward time is 100ms.
According to the method preparing mesohigh etched foil that technique scheme provides, adopt 3-4 electrolysis tank in secondary hair engaging aperture process, add the calcium polystyreme sulphonate of 0.01-0.03Wt% in tank liquor composition, current density 0.05-0.1A/cm
2.
According to the method preparing mesohigh etched foil that technique scheme provides, reprocessing adopts containing aluminum ions nitric acid weak solution, and concentration of nitric acid is 1-2Wt%, and aluminium ion concentration is 1-2Wt%.
Unless explicitly stated otherwise in contrast, otherwise all scopes that the present invention quotes comprise end value.Such as, " Mean Forward Current is 0.4-0.8A/cm
2" represent that the scope of Mean Forward Current is for being 0.4≤I≤0.8A/cm
2scope is 1.5≤W≤3.0.
Beneficial effect of the present invention is:
1) preparation method provided by the invention is on traditional sulfur process process base, pretreatment process is divided into two sections, alkali treatment and acid treatment, what in one-level hair engaging aperture process, employ pulse direct current superimposed current powers up forms of corrosion, the passivation of phosphoric acid,diluted overlay film was adopted before secondary chambering, use containing aluminum ions nitric acid weak solution in post-processing stages, the whole technological process of the method is simple, strong to corrosion tank liquor change adaptive, the corrosion hole uniform ground produced, improve the electrostatic specific volume of etched foil by a relatively large margin, there is comparatively excellent mechanical performance simultaneously, the hair engaging aperture process in traditional etching process of solving can not the restriction of power-off.
2) last process uses alkaline solution to dispel light paper tinsel surface and oil contaminant, dissolves surface film oxide, acquisition surface uniform, the aluminium foil that oxide-film is thinner;
3) intermediate pressure section 240Vf specific volume level can reach 2.5 μ F/cm
2, exceed 5-8% than conventional flat, pulling force 20-25N/cm, meet following process demand; High-pressure side 600Vf specific volume level is at 0.64 μ F/cm
2, exceed 3-6% than conventional flat, pulling force 22-26N/cm, meet following process demand; And in product appearance, because caloric value reduces, useless branch hole and uneven hole depth reduce, and the aberrations in property such as product appearance and specific volume is less, and production stability rises, the hair engaging aperture process in traditional etching process of improving greatly can not the restriction of power-off.
Accompanying drawing explanation
Fig. 1 is the current diagram in the embodiment of the present invention 1.
Fig. 2 is the current diagram in the embodiment of the present invention 2.
Fig. 3 is the current diagram in the embodiment of the present invention 3.
Embodiment
The following stated be the preferred embodiment of the present invention, what the present invention protected is not limited to following preferred implementation.It should be pointed out that on the basis of conceiving in these innovation and creation for a person skilled in the art, the some distortion made and improvement, all belong to protection scope of the present invention.Raw material used in embodiment all can be obtained by commercial sources.The industry standard of passing through is adopted to test, specific as follows:
Embodiment 1
Select Ruyuan Dongyangguang Fine Foil Co., Ltd. LC model 115 thickness light paper tinsel, its basic element is configured to Al>=99.99%, and other element kind and content thereof are Pb 0-1.0ppm, Zn 2-3ppm, Mg 3-7ppm, Cu 40-70ppm, Fe 5-15ppm, Si 5-25ppm; Through high-temperature vacuum stepped annelaing, make its cubic texture>=95%; 90Sec is soaked in 1mol/L sodium hydroxide solution at 35 DEG C; Put into the nitration mixture of 3Wt% sulfuric acid and 10Wt% nitric acid composition after washing, under the temperature conditions of 60 DEG C, process 120Sec; Carry out one-level hair engaging aperture after washing, electric current is for be about 0.5A/cm at single prescription wave impulse, forward duty ratio 60%, a Mean Forward Current
2, forward time 100ms basis on the permanent direct current of the lasting 10A of applying one, its current diagram is shown in accompanying drawing 1, adds galvano-cautery 65Sec at the temperature of 75 DEG C; Put into 5Wt% dilute phosphoric acid solution after washing, at 60 DEG C of temperature, process 120Sec; Paillon foil is put into second-level groove, and tank liquor composition proportion is the calcium polystyreme sulphonate of the nitric acid of 6Wt%, the aluminium ion of 0.2% and 0.01Wt%, uses the electrolysis tank of 2 V, at current density 0.1A/cm
2, electrochemical corrosion 8min (i.e. each V process 4min) under the condition that temperature is 65 DEG C; Put into the aluminium ion solution of 1-3Wt% nitric acid and 0.5-3Wt% after being washed by aluminium foil, at the temperature of 70 DEG C, process 4min; The air dry oven putting into 95 DEG C after washing processes 5min.
To the bending of obtained etched foil and specific volume method of testing as follows:
Bending is tested: test specimens size is 10mm*150mm (rushes sample burr and should be less than 0.1mm), use YAFENG company MIT-DA model bending tester, test condition knee radius of curvature R 1.0 ± 0.1mm, loading 2.5 ± 0.5N, angle of bend 90 ± 2 °, bending shuttle speed 6 times/S, upper and lower jaw separation 70 ± 2mm;
Specific volume is tested: use boric acid system to change into, being embodied in tank liquor is boric acid 100g/L, ammonium pentaborate 0.9g/L, resistivity 1650 ± 50 Ω cm, PH 3.5 ± 0.5, test specimens size is 500mm*10mm (rushes sample burr and should be less than 0.1mm), test solution is 70g/L, resistivity 7500 ± 300 Ω cm, temperature 70 ± 2 DEG C, PH 4.6 ± 0.5, measuring current 2 ± 0.2mA/ sheet.
The performance test of table 1 etched foil
| Experimental group | Bending/return | Specific volume/(μ F cm 2) | Thickness after corrosion/μm |
| 1-1 | 55 | 2.48 | 110 |
| 1-2 | 54 | 2.52 | 111 |
| 1-3 | 58 | 2.53 | 109 |
| 1-4 | 52 | 2.49 | 112 |
Embodiment 2
Xinjiang crowd is adopted to close G9 model 120 μm of thickness annealing light paper tinsels, cubic texture>=94%, its basic element is configured to Al>=99.98%, and other element kind and content thereof are Pb 0.8-1.2ppm, Zn 5-7ppm, Mg 1.5-2.5ppm, Cu 45-54ppm, Fe 11-14ppm, Si 15-17ppm, Ga 6-8ppm; In 1mol/L sodium hydroxide solution, at temperature 40 DEG C, soak 60Sec; Put into 5Wt% sulfuric acid solution after washing, under the temperature conditions of 60 DEG C, process 120Sec; At a list group triangular pulse after washing, forward duty ratio 70%, Mean Forward Current is about 0.5A/cm
2, the permanent direct current of the lasting 8A of applying one on the basis of forward time 100ms, its current diagram is shown in accompanying drawing 2, adds galvano-cautery 80Sec at the temperature of 72 DEG C; Put into 5Wt% dilute phosphoric acid solution after washing, at 60 DEG C of temperature, process 120Sec; Paillon foil is put into second-level groove, and tank liquor composition proportion is the calcium polystyreme sulphonate of the nitric acid of 8Wt%, the aluminium ion of 0.3% and 0.01Wt%, uses the electrolysis tank of 4 V, at current density 0.1A/cm
2, electrochemical corrosion 12min (i.e. each V process 3min) under the condition of temperature 70 C; Put into the aluminium ion solution of 1-3Wt% nitric acid and 0.5-3Wt% after being washed by aluminium foil, at the temperature of 70 DEG C, process 4min; The air dry oven putting into 95 DEG C after washing processes 5min.Method of testing is with embodiment 1, and test result is in table 2.
The performance test of table 2 etched foil
| Experimental group | Bending/return | Specific volume/(μ F cm 2) | Thickness after corrosion/μm |
| 2-1 | 58 | 0.634 | 112 |
| 2-2 | 56 | 0.662 | 111 |
| 2-3 | 54 | 0.641 | 112 |
| 2-4 | 52 | 0.642 | 113 |
Embodiment 3
Select light 1N99 model 110 thickness annealing light paper tinsel, cubic texture>=96%, its basic element is configured to Al>=99.98%, and other element kind and content thereof are Cu 55ppm, Fe 8-11ppm, Si 10-13ppm; In 0.5mol/L sodium hydroxide solution, at temperature 38 DEG C, soak 100Sec; Put into the nitration mixture of 5Wt% sulfuric acid and 4Wt% nitric acid composition after washing, under the temperature conditions of 55 DEG C, process 60Sec; Carry out one-level hair engaging aperture after washing, electric current is for be about 0.4A/cm at the profound wave impulse of Dan Zuzheng, forward duty ratio 60%, a Mean Forward Current
2, forward time 200ms basis on the permanent direct current of the lasting 15A of applying one, its current diagram is shown in accompanying drawing 3, adds galvano-cautery 70Sec at the temperature of 70 DEG C; Put into 5Wt% dilute phosphoric acid solution after washing, at 60 DEG C of temperature, process 120Sec; Paillon foil is put into second-level groove, and tank liquor composition proportion is the calcium polystyreme sulphonate of the nitric acid of 10Wt%, the aluminium ion of 0.5% and 0.05Wt%, uses the electrolysis tank of 3 V, at current density 0.1A/cm
2, electrochemical corrosion 9min (i.e. each V process 3min) under the condition that temperature is 65 DEG C; Put into the aluminium ion solution of 1-3Wt% nitric acid and 0.5-3Wt% after being washed by aluminium foil, at the temperature of 70 DEG C, process 4min; The air dry oven putting into 95 DEG C after washing processes 5min.Method of testing is with embodiment 1.
The performance test of table 3 etched foil
| Experimental group | Bending/return | Specific volume/(μ F cm 2) | Thickness after corrosion/μm |
| 3-1 | 48 | 0.852 | 111 |
| 3-2 | 52 | 0.862 | 110 |
| 3-3 | 56 | 0.841 | 113 |
| 3-4 | 52 | 0.856 | 112 |
As can be seen from the table, by the etched foil prepared by method of the present invention, there is good mechanical performance and higher specific volume.
Claims (8)
1. prepare a method for mesohigh etched foil with pulse direct current superimposed current, it is characterized in that, comprise the following steps:
A) last process: sodium hydroxide solution light paper tinsel raw material being put into 0.5-1mol/L, at 30-40 DEG C of process 60-120Sec;
B) the first two process: the above-mentioned aluminium foil through last process being put into concentration is 1-5Wt% sulfuric acid and 10-20Wt% nitric acid mixed solution, at 55-70 DEG C of process 90-120Sec;
C) one-level hair engaging aperture: the aluminium foil after the first two process above-mentioned is put into sulfuric acid, the hydrochloric acid of 3-5Wt%, the aluminum ions tank liquor of 1-2Wt% that concentration is 30-50Wt%, electrolysis 50-80Sec at 60-80 DEG C;
D) process in: the aluminium foil through hair engaging aperture step process is put into 3-5Wt% dilute phosphoric acid solution, at 55-65 DEG C of process 120-180Sec;
E) secondary hair engaging aperture: the aluminium foil processed in process is put into the calcium polystyreme sulphonate solution that tank liquor composition proportion is the nitric acid of 5-8Wt%, the aluminium ion of 0.2-0.5Wt% and 0.01-0.5Wt%, add electric treatment 12-18min at 65-80 DEG C of direct current;
F) reprocessing: put into by the aluminium foil through secondary hair engaging aperture containing 1-3Wt% nitric acid, the aluminum ions solution of 0.5-3Wt%, soaks 3-4min at 60-70 DEG C;
G) dry: the air dry oven that the aluminium foil through reprocessing puts into 80-120 DEG C is processed 2-5min, foil closing after drying.
2. the preparation method of mesohigh etched foil according to claim 1, is characterized in that, described smooth paper tinsel raw material are through the process of high-temperature vacuum stepped annelaing, thickness is 110-130 μm, the high-purity aluminum foil of cubic texture >=92%.
3. the preparation method of mesohigh etched foil according to claim 1, it is characterized in that, purity >=99.98% of described smooth paper tinsel raw material, wherein the content of impurity element Pb, Zn, Mg, Cu, Fe and Si is respectively 0-1.0ppm, 2-3ppm, 3-7ppm, 40-70ppm, 5-15ppm, 5-25ppm.
4. the preparation method of mesohigh etched foil according to claim 1, is characterized in that, is added with phosphide element and Ce elements in the treatment fluid of last process, and its content is respectively 60-90ppm and 20-40ppm.
5. the preparation method of mesohigh etched foil according to claim 1, is characterized in that, one-level hair engaging aperture apply the superimposed current that electric current is DC pulse.
6. the preparation method of mesohigh etched foil according to claim 1 or 5, it is characterized in that, described superimposed current increases a single group or many group pulse on the little galvanic basis of 10-20A, and wherein forward duty ratio is 50-80%, and Mean Forward Current is 0.4-0.8A/cm
2, the forward time is 100ms.
7. the preparation method of mesohigh etched foil according to claim 1, is characterized in that, adopts 3-4 electrolysis tank, add the calcium polystyreme sulphonate of 0.01-0.03Wt%, current density 0.05-0.1A/cm in tank liquor composition in secondary hair engaging aperture process
2.
8. the preparation method of mesohigh etched foil according to claim 1, is characterized in that, reprocessing adopts containing aluminum ions nitric acid weak solution, and concentration of nitric acid is 1-2Wt%, and aluminium ion concentration is 1-2Wt%.
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