CN101246779A - Production method of medium and high pressure formed foil - Google Patents
Production method of medium and high pressure formed foil Download PDFInfo
- Publication number
- CN101246779A CN101246779A CNA2008100657018A CN200810065701A CN101246779A CN 101246779 A CN101246779 A CN 101246779A CN A2008100657018 A CNA2008100657018 A CN A2008100657018A CN 200810065701 A CN200810065701 A CN 200810065701A CN 101246779 A CN101246779 A CN 101246779A
- Authority
- CN
- China
- Prior art keywords
- changes
- mesohigh
- acid
- foil
- paper tinsel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011888 foil Substances 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 22
- KGBXLFKZBHKPEV-UHFFFAOYSA-N Boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 19
- 239000004327 boric acid Substances 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 18
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 18
- 229910052708 sodium Inorganic materials 0.000 claims description 18
- 239000011734 sodium Substances 0.000 claims description 18
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 11
- 230000036571 hydration Effects 0.000 claims description 10
- 238000006703 hydration reaction Methods 0.000 claims description 10
- 238000009376 nuclear reprocessing Methods 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 238000005755 formation reaction Methods 0.000 claims description 6
- ABLZXFCXXLZCGV-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 6
- -1 phosphorous organic acid Chemical class 0.000 claims description 6
- VPTUPAVOBUEXMZ-UHFFFAOYSA-N (1-hydroxy-2-phosphonoethyl)phosphonic acid Chemical compound OP(=O)(O)C(O)CP(O)(O)=O VPTUPAVOBUEXMZ-UHFFFAOYSA-N 0.000 claims description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N Ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 4
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229950002499 Fytic acid Drugs 0.000 claims description 3
- GQZXNSPRSGFJLY-UHFFFAOYSA-N Hypophosphorous acid Chemical compound OP=O GQZXNSPRSGFJLY-UHFFFAOYSA-N 0.000 claims description 3
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 3
- 229940068041 Phytic Acid Drugs 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K [O-]P([O-])([O-])=O Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000000467 phytic acid Substances 0.000 claims description 3
- 235000002949 phytic acid Nutrition 0.000 claims description 3
- AQSJGOWTSHOLKH-UHFFFAOYSA-N Phosphite Chemical compound [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- BXLLINKJZLDGOX-UHFFFAOYSA-N dimethoxyphosphorylmethanamine Chemical class COP(=O)(CN)OC BXLLINKJZLDGOX-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical class [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 2
- 238000002161 passivation Methods 0.000 abstract description 34
- 238000000034 method Methods 0.000 abstract description 13
- 150000007524 organic acids Chemical class 0.000 abstract description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052698 phosphorus Inorganic materials 0.000 abstract 1
- 239000011574 phosphorus Substances 0.000 abstract 1
- 125000003703 phosphorus containing inorganic group Chemical group 0.000 abstract 1
- 238000002407 reforming Methods 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 description 16
- 229910052782 aluminium Inorganic materials 0.000 description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 15
- 239000011259 mixed solution Substances 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 230000002950 deficient Effects 0.000 description 6
- 230000002401 inhibitory effect Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000003068 static Effects 0.000 description 5
- 239000005030 aluminium foil Substances 0.000 description 4
- 230000000630 rising Effects 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000011031 large scale production Methods 0.000 description 3
- WNLRTRBMVRJNCN-UHFFFAOYSA-N Adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- ILRRQNADMUWWFW-UHFFFAOYSA-K Aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 2
- 210000003491 Skin Anatomy 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000002999 depolarising Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 230000002829 reduced Effects 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K Aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- ZRSKSQHEOZFGLJ-UHFFFAOYSA-N Ammonium adipate Chemical compound [NH4+].[NH4+].[O-]C(=O)CCCCC([O-])=O ZRSKSQHEOZFGLJ-UHFFFAOYSA-N 0.000 description 1
- 239000001741 Ammonium adipate Substances 0.000 description 1
- FEWJPZIEWOKRBE-XIXRPRMCSA-N Mesotartaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-XIXRPRMCSA-N 0.000 description 1
- ZADPBFCGQRWHPN-UHFFFAOYSA-N OBO Chemical compound OBO ZADPBFCGQRWHPN-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 235000019293 ammonium adipate Nutrition 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- ZRDXIILBYDTYOA-UHFFFAOYSA-N azane;phosphonous acid Chemical compound N.OPO ZRDXIILBYDTYOA-UHFFFAOYSA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 231100000078 corrosive Toxicity 0.000 description 1
- 231100001010 corrosive Toxicity 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000005712 crystallization Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing Effects 0.000 description 1
- 230000003628 erosive Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atoms Chemical class [H]* 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000003003 phosphines Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged Effects 0.000 description 1
- 229910052904 quartz Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 231100000486 side effect Toxicity 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- UKNAYQWNMMGCNX-UHFFFAOYSA-N sodium;[hydroxy(phenyl)methyl]-oxido-oxophosphanium Chemical class [Na+].[O-][P+](=O)C(O)C1=CC=CC=C1 UKNAYQWNMMGCNX-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229960001367 tartaric acid Drugs 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Abstract
The invention relates to a preparing method of a middle-high voltage formed foil, comprising the steps that: a middle-high voltage etched foil is put in pure water with a temperature no less than 96 DEG C to hydrate; the hydrated foil is electrified three to four levels to form; the formed foil is heated; the heated foil is put into the processing liquid including phosphorus-containing inorganic acid and/or phosphorus-containing organic acid to middle processing; the middle processed foil is put into the forming liquid to first reforming, with the same forming liquid as that of the second step; the first reformed foil is reheated; the reheated foil is second reformed; and the high-middle voltage formed foil is got. The invention has the advantages that: the passivation is highly effective, the passivant can be freely selected, the control scope of the parameter of the passivation is large, the processing process is more energy-saving and time-saving, as well as more suitable for current workshop scale production.
Description
Technical field
The present invention relates to a kind of preparation method of capacitor aluminium foil, more particularly, the present invention relates to the manufacture method of a kind of electrolytic capacitor with the mesohigh anode foils.
Background technology
Electrolytic capacitor is widely used in many relevant industries such as electronics.Now, scientific and technological progress and industrial expansion propose higher requirement to electrolytic capacitor in power frequency, Low ESR, long-life etc.In order to reach the higher electric property of electrolytic capacitor, in capacitor, often need to adopt the electrolyte of high moisture content, but, at high temperature, aluminum foil oxidation film is meeting of anode foils oxide-film and moisture generation aquation especially, thereby generate aluminium hydroxide on the anode foils surface, cause the decline of anode foils proof voltage, leakage current to increase, even can in capacitor, produce hydrogen, press liter in causing, shell drum shell and even quick-fried shell occur, have influence on electric property, the working life of electrolytic capacitor and even whole electric system, in addition safe in utilization.
For addressing the above problem, industry has extensively taked the passivation measure to prevent aluminum foil oxidation film and moisture generation aquation at present.Generally speaking, different with inhibition, the degree of passivation of water reaction to aluminium according to anion, general material can be divided into four classes promptly: unrestraint effect class, medium inhibitory action class, strong inhibitory action class and extremely strong inhibitory action class.And wherein, the aluminum orthophoshpate of generation is water insoluble, and the aluminum orthophoshpate structure on aluminum foil oxidation film surface is identical with the low quartz crystal formation, is stable positive tetrahedron crystalline texture, so phosphate radical belongs to the passivator of extremely strong inhibitory action class; The aluminum phosphate film has suppressed the effect of hydrated aluminum, having improved change into paper tinsel water-fast on apparent closes performance (its test mechanism shows as and surveys under the poach condition of back and directly under the poach condition, the time that extra electric field is set up voltage on fine and close aluminum phosphate film two sides is that pressure rising time is shorter), the pot-life that changes into paper tinsel and the working life of capacitor have been prolonged, in order to make the working life that improves capacitor, the mesohigh anode foils of high request adopts level Four to change into usually, and the general mesohigh anode foils that requires can adopt three grades to change into.
For this reason, industry normally adds a certain amount of Phos acids passivator such as phosphoric acid in the particular procedure tank liquor of chemical synthesis technology process at present, phosphorous acid, ortho phosphorous acid and its esters, or add a certain amount of organic phosphine acids passivator such as amino trimethylene methyl tri methylene phosphonic acid (ATMP), even carboxylic acid waits and carries out Passivation Treatment: promptly changing into after paper tinsel arrives maximum and become voltage (being commonly called as the seal making alive), etched foil inserted in the tank liquor that contains passivator soak certain hour, in the Passivation Treatment process, phosphoric acid or other acid groups have dissolved a part of pellumina, and the acid group on the passivator generates crystallization phosphating coat or alkyl reticular membrane on the pellumina surface.These film forming matters can make alumite that the aquation sensitivity is reduced, thereby the passivation of playing has improved the anti-hydrability that changes into paper tinsel and capacitor product thereof.
But existing Passivation Treatment has very important defective when enhancing product performance.At first, though it is straight hole shape hole that high pressure changes into the hole of paper tinsel, but the oxide-film that its surface generates still has certain thickness, passivator acid group or be difficult to fully diffuse into hole inside or when Passivation Treatment in conjunction with insecure, thus cause Passivation Treatment to be difficult to cover completely or destroyed easily comprehensively; And because Passivation Treatment efficient is lower, effect often improves concentration and temperature in order to reach preferably, and the static capacity of so easy loss part can not get both static capacity and anti-hydrability.
For addressing the above problem, it is that 200610063522.1 Chinese patent application discloses a kind of treatment process and method of inspection that suppresses aluminum foil for electrolytic condenser oxide-film and water reaction that application number is arranged, it is on existing aluminum foil for electrolytic condenser production technology (corrosion-cleaning one changes into) basis, increase the Passivation Treatment on aluminum foil oxidation film surface, its technology is: aluminium foil is after corrosion and clean technology, aluminium foil is flooded in containing the aqueous solution of phosphonium ion, clean and heat treatment through pure water again.But, the heat treatment of this technology is that 200 ℃-500 ℃ following processing times are 1h～3h in temperature, and the practical experience prompting: this heat treated burning sheet processing time is oversize, one comes the easy embrittlement of paillon foil, disconnected paper tinsel, or the paillon foil melting phenomenon takes place easily, unfavorable paillon foil oxide-film overall performance promotes, and the 2nd, heat treatment 1～3h power consumption, consuming time all too many.Obviously, this technical disadvantages is obvious, especially is difficult to realize large-scale production under existing workshop appliance, condition.
Also having application number is the manufacture method that 200610039699.8 Chinese patent application discloses a kind of electrode foil for aluminum electrolytic capacitors, press during it is got in the pure water of corrosive aluminum foil more than 95 degree reach and carry out hydration, after the hydration, soak in 40-80 0.1～5% ℃ the phosphoric acid solution, then carrying out secondary in the aqueous solution of 60～90 ℃ of the boric acid of the ammonium adipate of 0.5-3% and 3-10% changes into, after changing into for the first time, constant voltage 20-30 minute, and the high-temperature process by 350-500 ℃, after changing into for the second time, constant voltage 10～15 minutes.Between the Passivation Treatment that this technology is soaked phosphoric acid solution is arranged in hydration-treated and changes into, it is said that the electrode foil after the Passivation Treatment can improve specific volume 4-10%.But, the practical experience prompting: the water-repellent film performance of handling the paillon foil that obtains like this is not good, particularly along with formation voltage increases, serious curling can appear in paillon foil, and change into all variation of rear oxidation film electrical property and resistance to water, in a word, this technology does not possess practicality to the paillon foil that formation voltage surpasses 400V, is difficult to implement scale production under existing industry workshop appliance, condition yet.
Application number is 03139816.2 Chinese patent aluminum electrolysis capacitor anode foil manufacturing method in addition, comprise boiling pure water, change into, depolarising and change into processing again, change into electrolyte and comprise boronic acid containing or this type of inorganic acid of phosphoric acid or this type of organic acid of adipic acid, or the wherein at least a aqueous solution of their salt, in changing into electrolyte, the hypophosphorous acid, phosphorous acid, ortho phosphorous acid or its esters that add content and be 50ppm-5000ppm be as active material, and the citric acid, tartaric acid or its esters that add content and be 100ppm-10000ppm are as complexing agent.It is said: this method can resist the dissolving of paillon foil, helps reducing the decay of capacitance, thereby can make that capacitance is big, leakage current is less, resistance to water anode foil for aluminum electrolytic capacitor preferably.
Summary of the invention
Above-mentioned shortcoming at prior art; the objective of the invention is to provide a kind of mesohigh to change into the manufacture method of paper tinsel; this invention technical scheme has following advantage: Passivation Treatment efficient is higher; and passivator is selected, and the degree of freedom is big, the parameter control range elasticity of Passivation Treatment is big; processing procedure is more energy-conservation, save time, and is adapted to the workshop large-scale production of existing industry more.
For this reason, technical solution of the present invention is the manufacture method that a kind of mesohigh changes into paper tinsel, and it comprises the steps: A) mesohigh is corroded the pure water that paillon foil places temperature to be greater than or equal to 96 ℃ carry out hydration-treated; B) paillon foil after the hydration-treated being carried out three changes into to powering up of level Four; C) will heat-treat through the described paillon foil that changes into; D) will place treatment fluid to carry out processing through heat treated paillon foil, treatment fluid comprises inorganic phosphor-contained acid and/or phosphorous organic acid; E) paillon foil of handling in will passing through places and changes into liquid and carry out the 1st and change into, and the constituent that changes into liquid is identical with step B's; F) will carry out heat treatment once more through the 1st paillon foil that changes into again; G) will carry out the 2nd through heat treated paillon foil once more changes into again; H) obtain the finished product that described mesohigh changes into paper tinsel.
Traditional changes into and the Passivation Treatment process combined, as the disclosed technology of Chinese patent that application number is 200610063522.1, normally changes into the back in certain step and just and then carries out Passivation Treatment; Also have in this type of a kind of change into the typical process of Passivation Treatment combination as follows: boiling pure water → one-level changes into → secondary changes into → three grades change into → level Four changes into → heat treatment → 1st change into again → Passivation Treatment → 2nd change into again → heat treatment → 3rd changes into → Passivation Treatment → oven dry more again.Conventional art is as above just finished owing to change in that to change into step firm once finishing Passivation Treatment such as carrying out phosphoric acid, and the various defectives on the film all can't fix and present, simultaneously, loose oxide skin(coating) also may disturb passivation, and therefore, and then the passivation effect that carries out will be had a greatly reduced quality.And for example application number is 200610039699.8 the disclosed correlation technique of Chinese patent application, and then carries out the phosphoric acid Passivation Treatment after hydration, and similar shortcoming is equally also arranged.
The present invention observes originally and is found to the above-mentioned mechanism defective of traditional handicraft, creatively routine change into finish after, before the various defectives on the oxide-film all can't fix and present, do not carry out Passivation Treatment at once, but carry out heat treatment step earlier, utilize heat treatment high temperature, various defectives in changing into are all fixed and presented, and make loose oxide skin(coating) significantly disappear, thereby make the interference of passivation reduce, then carry out the impregnation process of passivating dip again: make passivator to carry out depolarising on the oxide-film surface pointedly, remedy the various defectives that are fixed and present, and impel and in changing into again subsequently, form firmer netted crystalline film., with the change into liquid that do not contain retarded acid replenish change into, make that various processing are just right and don't can produce the side effect of the undue erosion of retarded acid thereafter.Experiment showed, the paillon foil after the present invention handles, its passivation effect significantly promotes: the mesohigh paillon foil is water-fast to close that performance is better, specific volume also slightly promotes; And; because above-mentioned microcosmic mechanism advantage; method permission use kind of the present invention passivator is widely carried out Passivation Treatment and can both be reached the good water-fast effect of closing; simultaneously; permission is carried out elasticity control to the process parameters range in the Passivation Treatment; therefore, be adapted to the large-scale production in existing industry workshop more.
Because the inventive method is improved and above-mentioned microcosmic mechanism advantage, even the inventive method changes into for the aluminium foil of the highest withstand voltage aluminium dielectric capacitor, also can accomplish only to adopt the tertiary voltage distribution and needn't adopt the level Four voltage distribution, thereby saved the cost of energy consumption and production operation, the conventional art of comparing, the Passivation Treatment process of the inventive method can also be saved once and changes into except heat treatment time is shortened, thus also save time more, energy-conservation, efficient.
The manufacture method that mesohigh of the present invention changes into paper tinsel also further comprises following concrete improvement:
For obtaining better resultant effect, in the described steps A, described hydration-treated temperature more than 98 ℃, 6～15 minutes processing times.
Among the described step B, the described liquid that changes into is for containing the boric acid of 2～10 (wt%) and the aqueous solution of ammonium borate (sodium).
The described temperature that changes into liquid is 75～90 ℃, changes into to reach behind the ceiling voltage constant 10～30 minutes.
For guaranteeing passivation effect and excellent electrical and simplify the operation, described the 1st, 2 change into again change into the liquid proportioning, change into liquid temp, formation voltage is same as that afterbody changes among the described step B.
Described heat treatment, heat treated temperature all is controlled to be 400～520 ℃ once more, and the processing time is 1～4 minute.
Because the inventive method is improved and the advantage of microcosmic mechanism guarantees, the scope of choosing for deactivation matter is expanded promptly, in described step D, described inorganic phosphor-contained acid be phosphoric acid, phosphate, phosphorous acid, phosphite, hypophosphorous acid, hypophosphites one of them, described phosphorous organic acid be phytic acid, amino trimethyl phosphonic acids (ATMP), hydroxy ethylene diphosphonic acid (HEDP) one of them.
Because the inventive method is improved and the assurance of the advantage of microcosmic mechanism, also be expanded promptly for the control range of passivation operation, in described step D, the concentration of treatment fluid is 0.1～10g/L, temperature is 30～85 ℃, 2～15 minutes processing times.
For increasing the long-term storage performance of finished product, described manufacture method also comprises carries out reprocessing and oven dry with the 2nd paillon foil that changes into again.The ammonium dihydrogen phosphate of 2-6wt%, temperature 40-55 ℃, processing time 2-7 minute are adopted in described reprocessing; Described bake out temperature is 100～150 ℃ of scopes, and drying time is 2～7 minutes.
The present invention will be further described below in conjunction with specific embodiment.
Comparative example:
Adopt as etched foil same among the embodiment, poach is 12 minutes in the pure water more than 98 ℃, carries out the first order under 85 ℃ and change in the mixed solution of 5.0wt% boric acid, 1.0wt% ammonium borate (or sodium) aqueous solution, and constant voltage was 8 minutes when voltage arrived 200V; Then carry out the second level under 85 ℃ in the mixed solution of 5wt% boric acid, 0.5wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 10 minutes when voltage arrived 400V; Then carry out the third level under 85 ℃ in the mixed solution of 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 520V; Then carry out the fourth stage under 85 ℃ in the mixed solution of 5wt% boric acid, 0.08wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 30 minutes when voltage arrived 580V, then heat-treated, and temperature is 520 ℃, and the time is 2.5 minutes; Change at the above-mentioned fourth stage and to carry out the 1st in the liquid and change into again; Then carry out the phosphoric acid Passivation Treatment, solution concentration is that 6% (volume ratio), 65 ℃ of temperature, time are 6 minutes, cleans up the back and changes at the above-mentioned fourth stage and carry out the 2nd in the liquid and change into; Heat-treat, temperature is 500 ℃ again, and the time is 2.5 minutes; Change at the above-mentioned fourth stage and to carry out last changing in the liquid; Relevant electrical quantity is measured in oven dry at last, and measurement result sees Table 1.
Embodiment
Embodiment one:
Adopt the mesohigh etched foil, poach is 12 minutes in the pure water more than 98 ℃, and constant voltage is 10 minutes when then carrying out first order level formation voltage arrival 250V under 85 ℃ in the mixed solution of 5wt% boric acid, 0.3wt% ammonium borate (or sodium) aqueous solution; Then carry out the second level under 85 ℃ in 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 480V; Then carry out the third level under 85 ℃ in 5wt% boric acid, 0.08wt% ammonium borate (or sodium) mixed solution and change into, constant voltage was 30 minutes when voltage arrived 580V; Then heat-treat, temperature is 480 ℃, and the time is 2.5 minutes; Middle processing is carried out in the back in temperature is 45 ℃, 5g/L phosphoric acid solution, the time is 4.5 minutes; The back changes in the liquid the above-mentioned third level and changes into; Then carry out the heat treatment second time, temperature is 480 ℃, and the time is 2.5 minutes; Change into the above-mentioned third level and to carry out the 2nd in the liquid and change into, reprocessing adopts 4wt% ammonium dihydrogen phosphate, temperature to handle for 45 ℃, and the time is 4 minutes; Relevant electrical quantity is measured in oven dry at last.
Embodiment two:
Adopt the mesohigh etched foil, poach is 10 minutes in the pure water more than 98 ℃, then carries out first order level under 85 ℃ in the mixed solution of 6wt% boric acid, 0.2wt% ammonium borate (or sodium) aqueous solution and changes into, and constant voltage was 10 minutes when voltage arrived 250V; Then carry out the second level under 90 ℃ in 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 480V; Then carry out the third level under 90 ℃ in 5wt% boric acid, 0.08wt% ammonium borate (or sodium) mixed solution and change into, constant voltage was 30 minutes when voltage arrived 580V; Then heat-treat, temperature is 500 ℃, and the time is 2 minutes; Back temperature in the 2g/L phytic acid aqueous solution is 60 ℃, and the middle processing time is 6 minutes; The back changes in the liquid the above-mentioned third level and changes into; Then carry out the heat treatment second time, temperature is 500 ℃, and the time is 2 minutes; Change into the above-mentioned third level and to carry out the 2nd in the liquid and change into again; Relevant electrical quantity is measured in oven dry at last.
Embodiment three:
Adopt the mesohigh etched foil, poach is 12 minutes in the pure water more than 98 ℃, then carries out first order level under 85 ℃ in the mixed solution of 6wt% boric acid, 0.3wt% ammonium borate (or sodium) aqueous solution and changes into, and constant voltage was 10 minutes when voltage arrived 250V; Then carry out the second level under 85 ℃ in 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 480V; Then carry out the third level under 85 ℃ in 5wt% boric acid, 0.08wt% ammonium borate (or sodium) mixed solution and change into, constant voltage was 30 minutes when voltage arrived 580V; Then heat-treat, temperature is 500 ℃, and the time is 2.5 minutes; Back temperature in 1g/L ammonium hypophosphite solution is 70 ℃, and the middle processing time is 8 minutes; The back changes in the liquid the above-mentioned third level and changes into; Then carry out the heat treatment second time, temperature is 500 ℃, and the time is 2.5 minutes; Change into the above-mentioned third level and to carry out the 2nd in the liquid and change into, reprocessing adopts 4% phosphate, temperature to handle for 45 ℃, and the time is 6 minutes; Relevant electrical quantity is measured in oven dry at last.
Embodiment four:
Adopt the mesohigh etched foil, poach is 14 minutes in the pure water more than 98 ℃, then carries out first order level under 85 ℃ in the mixed solution of 6wt% boric acid, 0.3wt% ammonium borate (or sodium) aqueous solution and changes into, and constant voltage was 10 minutes when voltage arrived 250V; Then carry out the second level under 85 ℃ in 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 480V; Then carry out the third level under 85 ℃ in 5wt% boric acid, 0.08wt% ammonium borate (or sodium) mixed solution and change into, constant voltage was 30 minutes when voltage arrived 580V; Then heat-treat, temperature is 500 ℃, and the time is 2.5 minutes; Back temperature in the ATMP of 3g/L solution is 55 ℃, and the middle processing time is 4 minutes; The back changes in the liquid the above-mentioned third level and changes into; Then carry out the heat treatment second time, temperature is 500 ℃, and the time is 2.5 minutes; Change into the above-mentioned third level and to carry out the 2nd in the liquid and change into, reprocessing adopts 3wt% ammonium dihydrogen phosphate, temperature to handle for 50 ℃, and the time is 6 minutes; Relevant electrical quantity is measured in oven dry at last.
Respectively the paper tinsel that changes into of embodiment one to four, comparative example is tested, test event comprises static capacity, pressure rising time, resistance to water (survey back poach pressure rising time), and method of testing is tested by SJ/T 11140 standards, and test result is listed in the table 1.
Table 1
| Project | Pressure rising time (s) | Static capacity | Tr60(s) | 85 ℃ of life tests of capacitor |
| Comparative example | 158 | 100.0％ | 25 | Only reach 3000h |
| Embodiment one | 146 | 101.0％ | 12 | Reach 7000h |
| Embodiment two | 147 | 100.7％ | 15 | Reach 7000h |
| Embodiment three | 153 | 101.5％ | 11 | Reach 7000h |
| Embodiment four | 154 | 101.2％ | 13 | Reach 7000h |
As seen from the above table, the present invention makes change into paper tinsel water-fastly close the respective performances that performance and static capacity etc. all are better than traditional handicraft.
Claims (10)
1, a kind of mesohigh changes into the manufacture method of paper tinsel, and it comprises the steps: A) mesohigh is corroded the pure water that paillon foil places temperature to be greater than or equal to 96 ℃ carry out hydration-treated; B) paillon foil after the hydration-treated being carried out three changes into to powering up of level Four; C) will heat-treat through the described paillon foil that changes into; D) will place treatment fluid to carry out processing through heat treated paillon foil, treatment fluid comprises inorganic phosphor-contained acid and/or phosphorous organic acid; E) paillon foil of handling in will passing through places and changes into liquid and carry out the 1st and change into, and the constituent that changes into liquid is identical with step B's; F) will carry out heat treatment once more through the 1st paillon foil that changes into again; G) will carry out the 2nd through heat treated paillon foil once more changes into again; H) obtain the finished product that described mesohigh changes into paper tinsel.
2, mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: in the described steps A, described hydration-treated temperature more than 98 ℃, 6～15 minutes processing times.
3, mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: among the described step B, the described liquid that changes into is for containing the boric acid of 2～10 (wt%) and the aqueous solution of ammonium borate (sodium).
4, change into the manufacture method of paper tinsel as mesohigh as described in the claim 3, it is characterized in that: the described temperature that changes into liquid is 75～90 ℃, changes into to reach behind the ceiling voltage constant 10～30 minutes.
5, mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: described the 1st, 2 change into again change into the liquid proportioning, change into liquid temp, formation voltage is same as that afterbody changes among the described step B.
6, mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: described heat treatment, heat treated temperature all is controlled to be 400～520 ℃ once more, and the processing time is 1～4 minute.
7, mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: among the described step D, described inorganic phosphor-contained acid be phosphoric acid, phosphate, phosphorous acid, phosphite, hypophosphorous acid, hypophosphites one of them, described phosphorous organic acid be phytic acid, amino trimethyl phosphonic acids (ATMP), hydroxy ethylene diphosphonic acid (HEDP) one of them.
8, mesohigh changes into the manufacture method of paper tinsel according to claim 1, and it is characterized in that: among the described step D, the concentration of treatment fluid is 0.1～10g/L, and temperature is 30～85 ℃, 2～15 minutes processing times.
9, mesohigh changes into the manufacture method of paper tinsel according to claim 1, and it is characterized in that: described manufacture method also comprises carries out reprocessing and oven dry with the 2nd paillon foil that changes into again.
10, change into the manufacture method of paper tinsel as mesohigh as described in the claim 9, it is characterized in that: the ammonium dihydrogen phosphate of 2-6wt%, temperature 40-55 ℃, processing time 2-7 minute are adopted in described reprocessing; Described bake out temperature is 100～150 ℃ of scopes, and drying time is 2～7 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100657018A CN101246779B (en) | 2008-02-22 | 2008-02-22 | Production method of medium and high pressure formed foil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100657018A CN101246779B (en) | 2008-02-22 | 2008-02-22 | Production method of medium and high pressure formed foil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101246779A true CN101246779A (en) | 2008-08-20 |
| CN101246779B CN101246779B (en) | 2010-08-18 |
Family
ID=39947154
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100657018A Expired - Fee Related CN101246779B (en) | 2008-02-22 | 2008-02-22 | Production method of medium and high pressure formed foil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101246779B (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102610396A (en) * | 2011-01-20 | 2012-07-25 | 四川雅安艾华电极箔制造有限公司 | Manufacturing method for formed foil of electrolytic capacitor of energy-saving lamp |
| CN102891012A (en) * | 2012-09-14 | 2013-01-23 | 朱健雄 | Method for manufacturing amorphous oxidation film aluminum foil |
| CN106252081A (en) * | 2016-08-11 | 2016-12-21 | 四川立业电子有限公司 | A kind of anodizing composite dielectric film and preparation method thereof |
| CN107967996A (en) * | 2017-11-15 | 2018-04-27 | 广西贺州市桂东电子科技有限责任公司 | A kind of chemical synthesizing method of mash welder capacitor anode foils |
| CN108511195A (en) * | 2018-03-19 | 2018-09-07 | 南通海星电子股份有限公司 | A kind of post-processing approach improving middle-high voltage electrode foil coating mass |
| CN109859949A (en) * | 2018-01-26 | 2019-06-07 | 东莞东阳光科研发有限公司 | A method of reducing medium-high pressure chemical foil leakage current |
| CN110783107A (en) * | 2019-11-07 | 2020-02-11 | 南通海星电子股份有限公司 | Method for manufacturing high-mechanical-property low-voltage electrode foil |
| CN110959184A (en) * | 2017-07-28 | 2020-04-03 | 日本轻金属株式会社 | Electrode for aluminum electrolytic capacitor and method for producing same |
| CN110993347A (en) * | 2019-12-25 | 2020-04-10 | 西安交通大学 | High-voltage anode foil of sintered aluminum electrolytic capacitor and preparation method thereof |
| CN111146005A (en) * | 2019-12-25 | 2020-05-12 | 西安交通大学 | Sintered low-voltage anode foil of aluminum electrolytic capacitor and preparation method thereof |
| CN112119477A (en) * | 2018-05-17 | 2020-12-22 | 日本轻金属株式会社 | Method for manufacturing electrode for aluminum electrolytic capacitor |
| CN113611539A (en) * | 2021-07-13 | 2021-11-05 | 乳源县立东电子科技有限公司 | Low-voltage soft-state corrosion anode aluminum foil and preparation method and application thereof |
| CN113764191A (en) * | 2021-09-14 | 2021-12-07 | 南通海星电子股份有限公司 | An inhibitor for Al (OH)3Method for manufacturing low-voltage electrode foil formed by crystallization |
| CN113774456A (en) * | 2021-08-20 | 2021-12-10 | 扬州宏远电子股份有限公司 | Alternating-current corrosion foil formation process method for starting double-formation motor and aluminum foil |
-
2008
- 2008-02-22 CN CN2008100657018A patent/CN101246779B/en not_active Expired - Fee Related
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102610396A (en) * | 2011-01-20 | 2012-07-25 | 四川雅安艾华电极箔制造有限公司 | Manufacturing method for formed foil of electrolytic capacitor of energy-saving lamp |
| CN102610396B (en) * | 2011-01-20 | 2015-04-01 | 四川雅安艾华电极箔制造有限公司 | Manufacturing method for formed foil of electrolytic capacitor of energy-saving lamp |
| CN102891012A (en) * | 2012-09-14 | 2013-01-23 | 朱健雄 | Method for manufacturing amorphous oxidation film aluminum foil |
| CN106252081B (en) * | 2016-08-11 | 2019-01-29 | 四川立业电子有限公司 | A kind of anodizing composite dielectric film and preparation method thereof |
| CN106252081A (en) * | 2016-08-11 | 2016-12-21 | 四川立业电子有限公司 | A kind of anodizing composite dielectric film and preparation method thereof |
| CN110959184A (en) * | 2017-07-28 | 2020-04-03 | 日本轻金属株式会社 | Electrode for aluminum electrolytic capacitor and method for producing same |
| CN110959184B (en) * | 2017-07-28 | 2022-06-10 | 日本轻金属株式会社 | Electrode for aluminum electrolytic capacitor and method for producing same |
| CN107967996A (en) * | 2017-11-15 | 2018-04-27 | 广西贺州市桂东电子科技有限责任公司 | A kind of chemical synthesizing method of mash welder capacitor anode foils |
| CN109859949A (en) * | 2018-01-26 | 2019-06-07 | 东莞东阳光科研发有限公司 | A method of reducing medium-high pressure chemical foil leakage current |
| CN109859949B (en) * | 2018-01-26 | 2021-03-26 | 东莞东阳光科研发有限公司 | Method for reducing leakage current of medium-high voltage formed foil |
| CN108511195A (en) * | 2018-03-19 | 2018-09-07 | 南通海星电子股份有限公司 | A kind of post-processing approach improving middle-high voltage electrode foil coating mass |
| CN112119477B (en) * | 2018-05-17 | 2022-04-15 | 日本轻金属株式会社 | Method for manufacturing electrode for aluminum electrolytic capacitor |
| CN112119477A (en) * | 2018-05-17 | 2020-12-22 | 日本轻金属株式会社 | Method for manufacturing electrode for aluminum electrolytic capacitor |
| CN110783107A (en) * | 2019-11-07 | 2020-02-11 | 南通海星电子股份有限公司 | Method for manufacturing high-mechanical-property low-voltage electrode foil |
| CN110783107B (en) * | 2019-11-07 | 2021-06-29 | 南通海星电子股份有限公司 | Method for manufacturing high-mechanical-property low-voltage electrode foil |
| CN110993347A (en) * | 2019-12-25 | 2020-04-10 | 西安交通大学 | High-voltage anode foil of sintered aluminum electrolytic capacitor and preparation method thereof |
| CN111146005A (en) * | 2019-12-25 | 2020-05-12 | 西安交通大学 | Sintered low-voltage anode foil of aluminum electrolytic capacitor and preparation method thereof |
| CN113611539A (en) * | 2021-07-13 | 2021-11-05 | 乳源县立东电子科技有限公司 | Low-voltage soft-state corrosion anode aluminum foil and preparation method and application thereof |
| CN113611539B (en) * | 2021-07-13 | 2022-04-22 | 乳源县立东电子科技有限公司 | Low-voltage soft-state corrosion anode aluminum foil and preparation method and application thereof |
| CN113774456A (en) * | 2021-08-20 | 2021-12-10 | 扬州宏远电子股份有限公司 | Alternating-current corrosion foil formation process method for starting double-formation motor and aluminum foil |
| CN113764191A (en) * | 2021-09-14 | 2021-12-07 | 南通海星电子股份有限公司 | An inhibitor for Al (OH)3Method for manufacturing low-voltage electrode foil formed by crystallization |
| CN113764191B (en) * | 2021-09-14 | 2022-08-30 | 南通海星电子股份有限公司 | An inhibitor for Al (OH) 3 Method for manufacturing low-voltage electrode foil formed by crystallization |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101246779B (en) | 2010-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101246779B (en) | Production method of medium and high pressure formed foil | |
| CN101707142B (en) | Formation method for increasing hydration-proof performance of electrode foil for aluminum electrolytic capacitor | |
| CN106653373B (en) | A kind of aluminium electrolutic capacitor Waste Acid From Hua Cheng Foil and its production technology | |
| CN101110298B (en) | Method for manufacturing positive electrode aluminum foil of electrolytic capacitor | |
| CN101235529B (en) | Method for manufacturing low-pressure chemical synthesis foil for aluminum electrolysis capacitor and middle treatment groove | |
| CN102709059B (en) | Formation method for anode foil of intermediate-voltage aluminum electrolytic capacitor | |
| CN101425386A (en) | Preparation for producing aluminum electrolysis capacitor using ultrasonics | |
| CN101777432A (en) | Forming process of anode foils for extra-high voltage aluminium electrolytic capacitors | |
| CN104505260A (en) | Method for preparing mid-high voltage corrosion foil by using pulse DC superposed current | |
| CN102800483B (en) | Formation processing method for reducing leaking current of low-voltage formation foil | |
| CN103243369A (en) | Formation technique of medium/high-voltage anode aluminum foil for enhancing aluminum electrolytic capacitance | |
| CN101221855A (en) | Method for manufacturing formed foil used for medium-high pressure aluminum electrolytic capacitor | |
| JP2020507002A (en) | Chemical conversion method to reduce undulation of low pressure chemical conversion foil | |
| CN101707141A (en) | Method for manufacturing anodic foil of aluminum electrolytic capacitor | |
| CN100480427C (en) | Treating process inhibiting reaction between aluminium foil oxide film in electrolytic capacitor and water and inspection method thereof | |
| WO2019179185A1 (en) | Post-treatment method for improving quality of medium-high-voltage electrode foil oxide film | |
| CN110289171A (en) | A kind of manufacturing method of without phosphorus reaming aluminum electrolytic capacitor electrode foil | |
| CN104078240B (en) | Method for manufacturing anode foil of alternating current motor capacitor | |
| CN101748462A (en) | Formation method of anode aluminum foil for high-voltage aluminum electrolytic capacitor | |
| CN100587871C (en) | Production method of low pressure formed foil | |
| CN101425384B (en) | Low voltage aluminum electrolysis capacitor formed foil production method | |
| CN109786113A (en) | A kind of aluminium electrolutic capacitor Waste Acid From Hua Cheng Foil and its production technology | |
| CN110592637B (en) | Preparation method and application of formed foil | |
| CN101235527A (en) | Chemical synthesis method for anodic foil oxide film acid resistance | |
| CN101452768B (en) | Inspection method for inhibiting treatment process for reacting electrolytic capacitor aluminum foil oxidation film with water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100818 Termination date: 20200222 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |