CN109371399A - A kind of preparation method of corrosion-resistant aluminium and corrosion-resistant aluminium - Google Patents
A kind of preparation method of corrosion-resistant aluminium and corrosion-resistant aluminium Download PDFInfo
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- CN109371399A CN109371399A CN201811340575.2A CN201811340575A CN109371399A CN 109371399 A CN109371399 A CN 109371399A CN 201811340575 A CN201811340575 A CN 201811340575A CN 109371399 A CN109371399 A CN 109371399A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 100
- 239000004411 aluminium Substances 0.000 title claims abstract description 96
- 238000005260 corrosion Methods 0.000 title claims abstract description 76
- 230000007797 corrosion Effects 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000003990 capacitor Substances 0.000 claims abstract description 27
- 150000007524 organic acids Chemical class 0.000 claims abstract description 24
- 230000003068 static effect Effects 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 90
- 239000011888 foil Substances 0.000 claims description 89
- 235000010210 aluminium Nutrition 0.000 claims description 88
- 239000000243 solution Substances 0.000 claims description 82
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 54
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 235000006408 oxalic acid Nutrition 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- OXEDXHIBHVMDST-UHFFFAOYSA-N 12Z-octadecenoic acid Natural products CCCCCC=CCCCCCCCCCCC(O)=O OXEDXHIBHVMDST-UHFFFAOYSA-N 0.000 claims description 11
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 7
- 239000012670 alkaline solution Substances 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 6
- PYJJCSYBSYXGQQ-UHFFFAOYSA-N trichloro(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[Si](Cl)(Cl)Cl PYJJCSYBSYXGQQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005868 electrolysis reaction Methods 0.000 claims description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 230000003075 superhydrophobic effect Effects 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 11
- 150000002500 ions Chemical class 0.000 abstract description 5
- 230000004913 activation Effects 0.000 abstract description 2
- 230000004888 barrier function Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 36
- 235000019441 ethanol Nutrition 0.000 description 29
- 238000012360 testing method Methods 0.000 description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 21
- 229910001868 water Inorganic materials 0.000 description 14
- 238000001035 drying Methods 0.000 description 13
- 238000007605 air drying Methods 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 11
- 239000003643 water by type Substances 0.000 description 11
- 238000000605 extraction Methods 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 8
- -1 octadecylene Chemical group 0.000 description 8
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 7
- LLQHSBBZNDXTIV-UHFFFAOYSA-N 6-[5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-4,5-dihydro-1,2-oxazol-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC1CC(=NO1)C1=CC2=C(NC(O2)=O)C=C1 LLQHSBBZNDXTIV-UHFFFAOYSA-N 0.000 description 6
- 235000021355 Stearic acid Nutrition 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- KYIDJMYDIPHNJS-UHFFFAOYSA-N ethanol;octadecanoic acid Chemical compound CCO.CCCCCCCCCCCCCCCCCC(O)=O KYIDJMYDIPHNJS-UHFFFAOYSA-N 0.000 description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 6
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 6
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 6
- 239000008117 stearic acid Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 4
- 239000005711 Benzoic acid Substances 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 235000010233 benzoic acid Nutrition 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 235000019253 formic acid Nutrition 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 244000025254 Cannabis sativa Species 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 239000004310 lactic acid Substances 0.000 description 3
- 235000014655 lactic acid Nutrition 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 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
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- MMXKVMNBHPAILY-UHFFFAOYSA-N ethyl laurate Chemical compound CCCCCCCCCCCC(=O)OCC MMXKVMNBHPAILY-UHFFFAOYSA-N 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 230000009545 invasion Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010129 solution processing Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003211 malignant effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- ORYURPRSXLUCSS-UHFFFAOYSA-M silver;octadecanoate Chemical compound [Ag+].CCCCCCCCCCCCCCCCCC([O-])=O ORYURPRSXLUCSS-UHFFFAOYSA-M 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- LKOVPWSSZFDYPG-WUKNDPDISA-N trans-octadec-2-enoic acid Chemical compound CCCCCCCCCCCCCCC\C=C\C(O)=O LKOVPWSSZFDYPG-WUKNDPDISA-N 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
Abstract
The present invention relates to technical field of surface, disclose a kind of corrosion-resistant aluminium preparation method and corrosion-resistant aluminium, include the following steps: aluminium to be processed being put into organic acid soln, obtain the aluminium with micron coarse structure；Aluminium with micron coarse structure is put into low-surface-energy solution, obtains corrosion-resistant aluminium, wherein the static contact angle of corrosion-resistant aluminium material surface is not less than 150 °.By the present invention in that handling aluminium to be processed with organic acid soln, obtain the aluminium with micron coarse structure, it effectively prevent the foreign ions such as Cl- to corrode aluminium to be processed, the aluminium with micron coarse structure is then put into low-surface-energy solution, obtain super-hydrophobic corrosion-resistant aluminium, i.e. by carrying out surface super hydrophobic to aluminium to be processed, activation barrier potential of the aluminium to be processed in corrosion process can be improved, slow corrosion process is hindered, to achieve the purpose that improve its corrosion resistance, prolong its service life, promote aluminium electrolutic capacitor quality.
Description
Technical field
The present invention relates to technical field of surface, in particular to a kind of the preparation method and corrosion-resisting aluminium of corrosion-resistant aluminium
Material.
Background technique
It is pressurization of the aluminium flake after oxidation processes that the anode for being commercially used for aluminium electrolutic capacitor production at present, which draws foil,
There is the oxidation film of layer to have certain improvement on corrosion resistance compared to primary light foil for light foil, surface.But aluminium
There are a certain amount of water in electrolytic capacitor, water will form HCl solution with the Cl- in capacitor, easily invasion to alumina diaphragm defect
Place leads to the generation of anode extraction foil part acid corrosion, i.e. H2O+Cl-→HCl+HO-→HCl+Al+HO-→AlCl3+H2O or
H2O+Cl-→HCl+HO-→HCl+Al2O3+HO-→AlCl3+H2O, self-catalysis acid corrosion reaction meeting malignant development, finally leads
Cause capacitor failure.Therefore, water occurs in corrosion phenomenon to be a key factor in aluminium electrolyte capacitor, inhibits water to participate in rotten
Reaction process is lost, the corrosion resistance of aluminium electrolutic capacitor can be greatlyd improve, prolonged the service life.
In recent years, also further extensive for the research of material super hydrophobic surface in the prior art.Some researches show that,
Super hydrophobic surface is modified out in metal surface, water droplet can be made not assemble in metal surface, and in very small external force
Effect is lower can be so that water droplet be tumbled from super-hydrophobic metal surface.
Such as Chinese patent CN201610540625.6 discloses a kind of preparation method of super-amphiphobic layer surface aluminium flake, for
The marine environment problem serious to metal erosion, the patent by aluminium flake polishing, polishing, degreasing, oil removing, except using hydrochloric acid after passivation layer
Solution impregnates, and etches micron scale construction surface, then immerses in liquid nitrogen rapidly again after aluminium flake is immersed in boiling water, in the micron-scale
The enterprising step etching of body structure surface goes out nanoscale body structure surface, and surface micro-nano structure aluminium flake is immersed in the silver stearate of preparation
In, super-amphiphobic layer surface aluminium flake is made after drying.But since the aluminium flake in the patent is impregnated using hydrochloric acid solution,
Cl- will be remained in aluminum flake surface in this way, when being especially used for aluminium electrolutic capacitor, it will aggravate the corruption of aluminium electrolutic capacitor
Erosion reaction, and preparation method is complicated, higher cost.
In conclusion providing a kind of raising aluminium electrolutic capacitor corrosion resistance, prolonging the service life, preparation method letter
The problem of single, aluminium preparation method at low cost is current urgent need to resolve.
Summary of the invention
That the purpose of the present invention is to solve aluminium electrolutic capacitor poor corrosion resistance, service lifes in the prior art is short,
Preparation method is complicated, problem at high cost, and provide a kind of corrosion-resistant aluminium preparation method and corrosion-resistant aluminium.
In order to solve the above technical problems, including the following steps: the present invention provides a kind of preparation method of corrosion-resistant aluminium
Aluminium to be processed is put into organic acid soln, obtains the aluminium with micron coarse structure；
Aluminium with micron coarse structure is put into low-surface-energy solution, obtains corrosion-resistant aluminium, wherein corrosion-resisting aluminium
The static contact angle on material surface is not less than 150 °.
Compared with prior art, it by the present invention in that handling aluminium to be processed with organic acid soln, obtains thick with micron
The aluminium of rough structure, effectively prevent Cl-Equal foreign ions corrode aluminium to be processed, will then have a micron coarse structure
Aluminium be put into low-surface-energy solution, obtain super-hydrophobic corrosion-resistant aluminium, i.e., by aluminium to be processed carry out surface super hydrophobic
Change, activation barrier potential of the aluminium to be processed in corrosion process can be improved, hinders slow corrosion process, its is corrosion-resistant to reach raising
Performance, the purpose for prolonging its service life, promoting aluminium electrolutic capacitor quality, at the same time, since the preparation process is simple, also
Cost is saved.
Preferably, organic acid soln is oxalic acid solution.
Preferably, the concentration of organic acid soln is not less than 2M.
Preferably, the concentration range of organic acid soln is 2-3M.
Preferably, low-surface-energy solution be stearic acid ethanol solution, palmitinic acid ethanol solution, octadecenic acid ethanol solution,
Any one of octadecyl trichlorosilane alkane ethanol solution.
Preferably, low-surface-energy solution is octadecenic acid ethanol solution.
Preferably, further comprising the steps of before aluminium to be processed is put into organic acid soln: aluminium to be processed
It is put into alkaline solution.
Preferably, further comprising the steps of before aluminium to be processed is put into alkaline solution: successively by aluminium to be processed
After being put into acetone soln, ethanol solution, deionized water, then use ultrasonic cleaning.
The present invention provides a kind of corrosion-resistant aluminiums prepared by the preparation method by above-mentioned corrosion-resistant aluminium.
The application on foil is drawn in aluminum electrolysis capacitor anode in addition, the present invention also provides corrosion-resistant aluminiums.
Detailed description of the invention
One or more embodiments are illustrated by the picture in corresponding attached drawing, these exemplary theorys
The bright restriction not constituted to embodiment, the element in attached drawing with same reference numbers label are expressed as similar element, remove
Non- to have special statement, composition does not limit the figure in attached drawing.
Fig. 1 is schematic diagram of the water in the embodiment of the present invention 2 on super-hydrophobic corrosion-resistant anode extraction foil surface；
Fig. 2 is partial enlarged view at the A of Fig. 1；
Fig. 3 is the polarization curve of sample A, B.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with attached drawing to the present invention
Each embodiment be explained in detail.It will be understood by those skilled in the art that in various embodiments of the present invention, in order to
Reader is set to more fully understand the application and propose many technical details.But even if without these technical details and based on
Under each embodiment various changes and modifications, the application technical solution claimed also may be implemented.
Present embodiment is related to a kind of preparation method of corrosion-resistant aluminium, includes the following steps:
Aluminium to be processed is put into organic acid soln and is performed etching, the aluminium with micron coarse structure is obtained；
Aluminium with micron coarse structure is put into low-surface-energy solution to be surface modified, obtains corrosion-resistant aluminium,
The static contact angle of corrosion-resistant aluminium material surface is not less than 150 °.
Preferably, organic acid soln can be oxalic acid solution.
In a specific embodiment, the concentration of organic acid soln is not less than 2M, it is preferable that organic acid soln concentration range is
2-3M。
Preferably, low-surface-energy solution can be molten for stearic acid ethanol solution, palmitinic acid ethanol solution, octadecenic acid ethyl alcohol
Any one of liquid, octadecyl trichlorosilane alkane ethanol solution.
It should be noted that further including following before being put into aluminium to be processed and being performed etching in organic acid soln
Step: aluminium to be processed is put into alkaline solution to remove the oxide layer of aluminium material surface to be processed.Specifically, when aluminium to be processed is
When anode in aluminium electrolutic capacitor draws foil, since anode draws the oxidation film that there is layer on foil surface, need wait locate
Reason aluminium is put into alkaline solution before reacting with organic acid soln to remove the oxide layer of aluminium material surface to be processed.Certainly, wait locate
Reason aluminium be also possible to the aluminium that surface does not form oxide layer, when not forming oxide layer, can directly by its with it is organic
Acid solution is reacted.
In addition, the preparation method is further comprising the steps of before aluminium to be processed is put into alkaline solution:
After aluminium to be processed is sequentially placed into acetone soln, ethanol solution, deionized water, then use ultrasonic cleaning 5min
To remove the surface residues of aluminium to be processed.Specifically, which is gone using chemicals such as acetone soln, ethanol solutions
Except the grease and other impurities of aluminium material surface to be processed.
Specifically, the preparation method for drawing foil to corrosion-resistant anode is described in detail:
Test material: common 650VF anode to be processed draws foil, acetone, ethyl alcohol, deionized water, sodium hydroxide, grass
Acid, stearic acid.
Test apparatus: supersonic wave cleaning machine, beaker
In present embodiment, 12 embodiments will be provided as follows.
It 12 common 650VF anodes to be processed is drawn into foils is sequentially placed into and be respectively provided with acetone, ethyl alcohol, deionized water
In clean beaker, and it is placed in progress each 5min of ultrasonic cleaning in supersonic wave cleaning machine；
Foil will be drawn by treated anode to take out, it is stand-by after natural drying 10min；
A clean beaker is taken to prepare 1M sodium hydroxide solution 200ml, the oxalic acid of another compound concentration 2M, 2.5M, 3M respectively are molten
Liquid 100ml is stand-by；
The anode after drying is first drawn into foil and immerses 1M sodium hydroxide solution to remove surface oxide layer, after 10min simultaneously
It takes out and cleans simultaneously natural air drying with a large amount of deionized waters；12 anodes after air-drying are drawn into foil again and are divided into 3 groups, are immersed respectively
To construct surface roughness, process continues 5min, is drawn after the completion with a large amount of deionized waters to anode the oxalic acid of 2M, 2.5M, 3M
Foil cleaning and natural air drying out；
Taking a clean beaker to prepare mass fraction respectively is 1% stearic acid ethanol solution, palmitinic acid ethanol solution, octadecylene
Sour ethanol solution, octadecyl trichlorosilane alkane ethanol solution 200ml；Every group of anode after drying is drawn into foil and is respectively placed in preparation
Good stearic acid ethanol solution, palmitinic acid ethanol solution, octadecenic acid ethanol solution, in octadecyl trichlorosilane alkane ethanol solution
10min, the property for drawing foil surface low-surface-energy the purpose is to assign anode；
Anode is taken out after the completion of above-mentioned steps and draws foil, is rinsed to remove remaining solution, then with a large amount of deionized waters
It air-dries and obtains corrosion-resistant anode extraction foil.
Through surface static contact angle test, 12 anodes draw the static contact angle and corresponding acidizer, low table of foil
Face energy solution is as shown in table 1:
The treatment conditions and static contact angle test number of 1 12 embodiments of table
| Serial number | Concentration of oxalic acid (M) | Low-surface energy substance classification | Static contact angle numerical value |
| Embodiment 1 | 2 | Stearic acid | 155° |
| Embodiment 2 | 2 | Palmitinic acid | 152° |
| Embodiment 3 | 2 | Octadecenic acid | 164° |
| Embodiment 4 | 2 | Octadecyl trichlorosilane alkane | 162° |
| Embodiment 5 | 2.5 | Stearic acid | 154° |
| Embodiment 6 | 2.5 | Palmitinic acid | 153° |
| Embodiment 7 | 2.5 | Octadecenic acid | 165° |
| Embodiment 8 | 2.5 | Octadecyl trichlorosilane alkane | 163° |
| Embodiment 9 | 3 | Stearic acid | 157° |
| Embodiment 10 | 3 | Palmitinic acid | 154° |
| Embodiment 11 | 3 | Octadecenic acid | 167° |
| Embodiment 12 | 3 | Octadecyl trichlorosilane alkane | 165° |
The static contact angle of super hydrophobic surface is more than or equal to 150 °, just has good hydrophobic performance, as seen from the above table, warp
The angle that 12 anodes that the method for crossing 12 embodiments of present embodiment is handled draw the static contact angle of foil is all larger than
150 °, i.e., the surface that 12 anodes draw foil has been carried out super-hydrophobicization, has good corrosion resistance.
About Corrosion Resistant Mechanism, as depicted in figs. 1 and 2, the coarse structure that super-hydrophobic corrosion-resistant anode draws 1 surface of foil is deposited
In a large amount of holes, therefore in impregnation process, these holes can capture gas, draw 1 surface shape of foil in super-hydrophobic corrosion-resistant anode
At the film layer of one layer similar " mattress ", as corrosion 2 (such as H of drop2O、Cl-) by super-hydrophobic corrosion-resistant anode extraction 1 surface of foil
When, due to the influence of rough porosity thereon, the air cushion 3 on surface will completely cut off contact with corrosive deposit, improve corrosion resistance.
In the present embodiment, 12 embodiments handle anode to be processed by using oxalic acid solution and draw foil, are had
There is the anode of micron coarse structure to draw foil, effectively prevent Cl-Equal foreign ions are drawn foil to anode to be processed and are corroded, and
Foil will be drawn with the anode of micron coarse structure afterwards and is put into low-surface-energy solution, obtain super-hydrophobic corrosion-resistant anode and draw foil,
Surface super hydrophobic is carried out by drawing foil to anode to be processed, the corrosion resistance that anode draws foil surface can be promoted,
To assign aluminium electrolutic capacitor corrosion resistance more excellent under high-temperature high-load.
Comparative example one is selected about organic acid
This group of comparative example uses lactic acid solution, formic acid solution, acetum, benzoic acid solution processing anode to draw respectively
Foil, then by identical low-surface-energy solution processing after, carry out surface static contact angle test, and with embodiment 1 into
Row comparison, the specific steps are as follows:
Test material: common 650VF anode to be processed draws foil, acetone, ethyl alcohol, deionized water, sodium hydroxide, cream
Acid, formic acid, acetic acid, benzoic acid, stearic acid.
Test apparatus: supersonic wave cleaning machine, beaker
It takes the same batch of multistage, common 650VF anode to be processed to draw foil, is denoted as comparative example 1-4, is sequentially placed into and fills respectively
Have acetone, ethyl alcohol, deionized water clean beaker in, and be placed in supersonic wave cleaning machine progress each 5min of ultrasonic cleaning,
The purpose is to the grease and other impurities on its surface are removed by chemical；
Foil will be drawn by treated comparative example 1-4 anode to take out, it is stand-by after natural drying 10min；
It takes a clean beaker to prepare 1M sodium hydroxide solution 200ml, separately prepares lactic acid solution, the formic acid of same concentration 2M respectively
Each 100ml of solution, acetum, benzoic acid solution is stand-by；
First by the anode extraction foil immersion 1M sodium hydroxide solution of the comparative example 1-4 after drying to remove surface oxide layer,
It is taken out simultaneously after 10min and cleans simultaneously natural air drying with a large amount of deionized waters；1 anode of comparative example after air-drying is drawn into foil leaching again
Enter 2M lactic acid solution, 2 anode of comparative example draw foil immerse 2M formic acid solution, 3 anode of comparative example draw foil immerse 2M acetum,
4 anode of comparative example draws foil and immerses 2M benzoic acid solution to construct surface roughness, and process continues 5min, after the completion with a large amount of
The anode of deionized water comparative example 1-4 draws foil cleaning and natural air drying；
Taking a clean beaker to prepare mass fraction is 1% stearic ethanol solution 200ml；By the comparative example 1- after drying
4 anode draws foil and is placed in 10min in prepared stearic acid ethanol solution, and the purpose is to assign anode to draw the low table in foil surface
The property of face energy；
The anode that comparative example 1-4 is taken out after the completion of above-mentioned steps draws foil, is rinsed with a large amount of deionized waters to remove residual
Solution, then air-dry.
Through surface static contact angle test, the anode of comparative example 1-4 draw foil contact angle and corresponding acidizer and
It is as shown in table 2 with the comparison of embodiment 1:
2 comparative example 1-4 of table and the static contact angle of embodiment 1 compare
As seen from the above table, remaining four kinds of organic acid selected by comparative example after being processed, draw what foil obtained in anode
Static contact angle is below 150 °, it is seen then that not all organic acid can meet processing requirement of the invention.
Comparative example two is selected about concentration of oxalic acid
This group of comparative example is drawn foil to anode using the oxalic acid solution of various concentration and is surface-treated, and then carries out static
The test of contact angle, and compared with embodiment 1, the preparation method of this comparative example is same as Example 1, specific to walk
It is rapid as follows:
Test material: common 650VF anode to be processed draws foil, acetone, ethyl alcohol, deionized water, sodium hydroxide, grass
Acid, stearic acid.
Test apparatus: supersonic wave cleaning machine, beaker
Test procedure:
It takes the same batch of multistage, anode to be processed to draw foil, is denoted as comparative example 5, comparative example 6, is sequentially placed into and is respectively provided with
Acetone, ethyl alcohol, deionized water clean beaker in, and be placed in supersonic wave cleaning machine progress each 5min of ultrasonic cleaning,
Purpose is the grease and other impurities that its surface is removed by chemical；
It is taken out foil is drawn by the anode of treated comparative example 5-6, it is stand-by after natural drying 10min；
A clean beaker is taken to prepare 1M sodium hydroxide solution 200ml, the oxalic acid solution for separately preparing various concentration respectively is each
100ml is stand-by, and concentration is followed successively by 1M, 1.5M.
First by the comparative example 5-6 anode extraction foil immersion 1M sodium hydroxide solution after drying to remove surface oxide layer,
It is taken out simultaneously after 10min and cleans simultaneously natural air drying with a large amount of deionized waters；5 anode of comparative example after air-drying is drawn into foil leaching again
Enter 1M oxalic acid solution, comparative example 6 foil immerse 1.5M oxalic acid solution to construct surface roughness, process continues 5min, completion
Simultaneously natural air drying is cleaned with foil of a large amount of deionized waters to comparative example 5-6 afterwards.
Taking a clean beaker to prepare mass fraction is 1% stearic ethanol solution 200ml；By the comparative example 5- after drying
6 anodes draw foil and are placed in 10min in prepared stearic acid ethanol solution, and the purpose is to assign anode to draw the low surface in foil surface
The property of energy；
Comparative example 5-6 anode is taken out after the completion of above-mentioned steps and draws foil, is rinsed with a large amount of deionized waters remaining to remove
Then solution air-dries.
Through surface static contact angle test, comparative example 5-6 anode draw foil contact angle and corresponding concentration of oxalic acid and with reality
The comparison for applying example 1 is as shown in table 3:
3 comparative example 5-6 of table and the static contact angle of embodiment 1 compare
It is handled it can be seen from numerical value in table even with oxalic acid, is also there is its concentration compared with strict requirements, concentration
When low, the problem to be solved in the present invention not can solve, wherein the concentration of the 2M of embodiment 1 is critical value, and the concentration lower than 2M reaches
Less than present invention technical effect to be achieved.
Comparative example three is selected about low-surface-energy solution
This group of comparative example is drawn foil to anode using different types of low-surface-energy solution and is surface-treated, and then carries out
The test of Static Contact angle, and compared with embodiment 1, the preparation method of this comparative example is same as Example 1, specific to walk
It is rapid as follows:
Test material: common 650VF anode to be processed draws foil, acetone, ethyl alcohol, deionized water, sodium hydroxide, grass
Acid, lauric acid, palmitinic acid, octadecenic acid, octadecyl trichlorosilane alkane；
Test apparatus: supersonic wave cleaning machine, beaker；
Test procedure:
Take the same batch of multistage, anode to be processed to draw foil, be denoted as comparative example 7-10, be sequentially placed into be respectively provided with acetone,
Ethyl alcohol, deionized water clean beaker in, and be placed in supersonic wave cleaning machine progress each 5min of ultrasonic cleaning, the purpose is to
The grease and other impurities on its surface are removed by chemical；
It is taken out foil is drawn by the anode of treated comparative example 7-10, it is stand-by after natural drying 10min；
A clean beaker is taken to prepare 1M sodium hydroxide solution 200ml, another clean beaker prepares the oxalic acid solution 100ml of 2M
For use；
First by the anode extraction foil immersion 1M sodium hydroxide solution of the comparative example 7-10 after drying to remove surface oxide layer,
It is taken out simultaneously after 10min and cleans simultaneously natural air drying with a large amount of deionized waters；The comparative example 7-10 anode after air-drying is drawn again
Foil immerses 2M oxalic acid solution to construct surface roughness, and process continues 5min, after the completion with a large amount of deionized waters to No. 11-15
Foil cleaning and natural air drying；
Clean beaker is taken to prepare the ethyl laurate solution 100ml that mass fraction is 1%, palmitinic acid ethanol solution respectively
100ml, octadecenic acid ethanol solution 100ml, octadecyl trichlorosilane alkane ethanol solution 100ml；By the comparative example 7- after drying
10 extraction foil is respectively placed in 10min in prepared above-mentioned low-surface-energy solution, and the purpose is to assign anode to draw foil surface
The property of low-surface-energy；
The anode that comparative example 7-10 is taken out after the completion of above-mentioned steps draws foil, is rinsed with a large amount of deionized waters to remove residual
Solution, then air-dry.
Through surface static contact angle test, comparative example 7-10 anode draw foil contact angle and corresponding dressing agent and with reality
The comparison for applying example 1 is as shown in table 4:
4 comparative example 7-10 of table and the static contact angle of embodiment 1 compare
By table 4 as it can be seen that selected low-surface energy substance plays the role of dropping low-surface-energy, but because of low-surface energy substance institute itself
Difference containing carbon chain lengths and functional group, modification effect also have difference, increase from the results of view with dressing agent carbochain, to sun
The super-hydrophobic modification effect that foil surface is drawn in pole is also better；When carbon chain lengths are identical, containing functional group, (such as alkenyl, chlorine replace
Base) low-surface energy substance such as octadecenic acid and octadecyl trichlorosilane alkane modification effect it is more excellent, but from avoid introduce chloride ion
Impurity considers, it is preferable to use octadecenic acid.Therefore, and the processing of not all low-surface energy substance can solve technology of the invention
Problem
Test and comparative example
Choose respectively it is unprocessed, through the embodiment of the present invention 1, embodiment 3 and the prior art using inorganic acid (hydrochloric acid)
The aluminum electrolysis capacitor anode of processing draws after foil is assembled into capacitor and carries out life test and corrosion resistance verifying, specifically such as
Under:
The specification of aluminium electrolutic capacitor is 420V, 680 μ F, 35 Φ × 50mm；Above-mentioned all aluminium electroloysis simultaneously
The Working electrolyte that capacitor uses is all self-control, and other materials is all identical.Common anode is used to draw foil (untreated) as system
It is P group that the product of work, which is compiled, and being drawn aluminium electrolutic capacitor made by foil using anode prepared by oxalic acid and compiled is N group, uses hydrochloric acid
It is S group that the anode of preparation, which is drawn aluminium electrolutic capacitor made by foil and compiled,.P group, N group and S group is each selects 6 products, measurement is initial
Direct current is carried out after parameter adds ripple load life to test.Experimental condition are as follows: 105 DEG C, 120Hz, ripple current 3.28A/pcs,
Voltage rating full load throws examination.Parameter testing temperature is 25 DEG C, and humidity 45%, data are averaged.
Firstly, as shown in figure 3, being carried out by electrochemical workstation to above-mentioned untreated samples (A), 3 sample of embodiment (B)
TAFEL curve test, the aqueous solution that test solution is 0.5M NaCl+0.1M HCl.By comparing two sample foils in analysis chart
Polarization curve, it is evident that the corrosion potential of 3 sample of embodiment (B) is greater than untreated samples (A), corrosion current
Less than untreated samples (A), Pitting Potential is also above untreated samples (A), it can be seen that embodiment 3 from polarization curve
Sample (B) is than untreated samples (A) more resistant to electrochemical corrosion.
Secondly, life of product and corrosion condition test result are as shown in table 5:
The test of table 5 and comparative example life of product and corrosion condition test result
By table 5 as it can be seen that by 105 DEG C, after 5000H life test, the capacitor of foil preparation is drawn using untreated anode
There is corrosion phenomenon in discovery after (P group) disintegrates, and corrosion probability is up to 83.3%, and the variation of product parameters is obvious；Wherein exist
There is product (P3) leakage without capacity in 4000H, and the discovery anode that disintegrates draws foil and heavy corrosion occurs.
There is a production in discovery after being disintegrated using the capacitor (N group) that the method processing anode of embodiment 1 draws foil preparation
There is slight erosion in product (N2), other products do not corrode, and product parameters change rate is significantly less than P group.Using oxalic acid system
Standby anode draws the aluminium electrolutic capacitor of foil production after 105 DEG C, 5000H life test, and product capacity decaying obviously subtracts
Small, loss and leakage current amplification obviously lower.Product corrosion probability is only 16.7%, compared to common anode draw foil product and
The product of HCl treatment, which has, significantly to be reduced.
The anode prepared using hydrochloric acid draws the aluminium electrolutic capacitor (S group) of foil production after same life test,
There is 50% product the case where heavy corrosion fracture occur, and product rate of corrosion is also up to 83.3%.
For the prior art using hydrochloric acid handled as a result, being because wherein containing the acidizer of chlorine, hydrochloric acid makes
With inevitably anode draw foil gap between remained Cl-, and in sour treatment process, the water in air also has micro residual
It stays between gap；Although anode draws foil surface and good super-hydrophobicity is presented after low-surface-energy is handled, inside is already invaded
Foreign ion Cl is entered-, the corrosion inside anode extraction foil is exacerbated with internal moisture collective effect, and then lead to product
Generation of the leakage without capacity.
In conclusion the anode handled using the non-organic acid containing chlorine draws foil, to anode to be processed draw foil into
Row surface super hydrophobic can form better corrosion-resistant film layer, effectively obstruct miscellaneous in water or other supplementary materials in electrolyte
Matter ion (such as Cl-Deng) corrosion invasion, thus promoted anode draw foil corrosion resistance；Using the aluminium electroloysis electricity of its production
Container products corrosion resistance is obviously improved, and extends the service life of aluminium electrolutic capacitor.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of the claim
Subject to enclosing.
Claims (10)
1. a kind of preparation method of corrosion-resistant aluminium, which comprises the steps of:
Aluminium to be processed is put into organic acid soln, obtains the aluminium with micron coarse structure；
The aluminium with micron coarse structure is put into low-surface-energy solution, obtains corrosion-resistant aluminium,
The static contact angle of the corrosion-resistant aluminium material surface is not less than 150o.
2. the preparation method of corrosion-resistant aluminium according to claim 1, it is characterised in that: the organic acid soln is oxalic acid
Solution.
3. the preparation method of corrosion-resistant aluminium according to claim 2, it is characterised in that: the concentration of the organic acid soln
Not less than 2M.
4. the preparation method of corrosion-resistant aluminium according to claim 3, it is characterised in that: the concentration of the organic acid soln
Range is 2-3M.
5. the preparation method of corrosion-resistant aluminium according to claim 1, it is characterised in that: the low-surface-energy solution is hard
Resin acid ethanol solution, palmitinic acid ethanol solution, octadecenic acid ethanol solution, any in octadecyl trichlorosilane alkane ethanol solution
Kind.
6. the preparation method of corrosion-resistant aluminium according to claim 5, it is characterised in that: the low-surface-energy solution 18
Olefin(e) acid ethanol solution.
7. the preparation method of described in any item corrosion-resistant aluminiums according to claim 1~6, it is characterised in that: will be to be processed
Aluminium be put into organic acid soln before, it is further comprising the steps of:
The aluminium to be processed is put into alkaline solution.
8. the preparation method of corrosion-resistant aluminium according to claim 7, it is characterised in that: put by the aluminium to be processed
It is further comprising the steps of before entering alkaline solution:
After the aluminium to be processed is sequentially placed into acetone soln, ethanol solution, deionized water, then use ultrasonic cleaning.
9. a kind of corrosion-resistant aluminium prepared by the preparation method by the described in any item corrosion-resistant aluminiums of the claims 1-8.
10. the described in any item corrosion-resistant aluminiums of claim 1-8 draw the application on foil in aluminum electrolysis capacitor anode.
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