CN107452518B - Reduce the chemical synthesizing method of medium-high pressure chemical foil leakage current - Google Patents
Reduce the chemical synthesizing method of medium-high pressure chemical foil leakage current Download PDFInfo
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- CN107452518B CN107452518B CN201710682543.XA CN201710682543A CN107452518B CN 107452518 B CN107452518 B CN 107452518B CN 201710682543 A CN201710682543 A CN 201710682543A CN 107452518 B CN107452518 B CN 107452518B
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- 239000000126 substance Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000011888 foil Substances 0.000 title claims abstract description 21
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 18
- 239000005030 aluminium foil Substances 0.000 claims abstract description 83
- 239000007864 aqueous solution Substances 0.000 claims abstract description 52
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 26
- 229940067597 azelate Drugs 0.000 claims abstract description 25
- JOPDZQBPOWAEHC-UHFFFAOYSA-H tristrontium;diphosphate Chemical compound [Sr+2].[Sr+2].[Sr+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JOPDZQBPOWAEHC-UHFFFAOYSA-H 0.000 claims abstract description 20
- 239000004327 boric acid Substances 0.000 claims abstract description 18
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- OCLWYHKNYKCKHU-UHFFFAOYSA-N nonanedioic acid;sodium Chemical compound [Na].OC(=O)CCCCCCCC(O)=O OCLWYHKNYKCKHU-UHFFFAOYSA-N 0.000 claims description 19
- 238000007598 dipping method Methods 0.000 claims description 11
- 230000003628 erosive effect Effects 0.000 claims description 11
- 230000005611 electricity Effects 0.000 claims description 6
- 229910052738 indium Inorganic materials 0.000 claims description 5
- UYEMGAFJOZZIFP-UHFFFAOYSA-N 3,5-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC(O)=CC(O)=C1 UYEMGAFJOZZIFP-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 2
- UDOPWDMIGDFPBW-UHFFFAOYSA-N nonanedioic acid;potassium Chemical compound [K].OC(=O)CCCCCCCC(O)=O UDOPWDMIGDFPBW-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 25
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000002791 soaking Methods 0.000 abstract 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid group Chemical group C(CCCCC(=O)O)(=O)O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 13
- 239000007788 liquid Substances 0.000 description 11
- 229910021538 borax Inorganic materials 0.000 description 8
- 239000004328 sodium tetraborate Substances 0.000 description 8
- 235000010339 sodium tetraborate Nutrition 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 229960000250 adipic acid Drugs 0.000 description 6
- 235000011037 adipic acid Nutrition 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 5
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- -1 phosphate dihydrogen salt Chemical class 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 125000005619 boric acid group Chemical group 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
- H01G13/06—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00 with provision for removing metal surfaces
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/055—Etched foil electrodes
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Cell Electrode Carriers And Collectors (AREA)
Abstract
The invention discloses a kind of chemical synthesizing methods for reducing medium-high pressure chemical foil leakage current, it is placed in azelate aqueous solution including soaking aluminium foil in water, carry out level-one chemical conversion, first wash is carried out later, then aluminium foil is placed in azelate aqueous solution, carry out second level chemical conversion, second wash, aluminium foil is placed in azelate aqueous solution again, carry out three-level chemical conversion, aluminium foil after three-level chemical conversion chemical conversion is placed in 3, it is impregnated in 5- dihydroxy-benzoic acid aqueous solution, high-temperature heat treatment, aluminium foil after high-temperature process is placed in again in the aqueous solution of boric acid and strontium phosphate, carry out level Four chemical conversion, high-temperature heat treatment, aluminium foil is finally placed in Pyatyi in boric acid and strontium phosphate aqueous solution to be melted into, it is subsequently placed in after being impregnated in phosphoric acid solution and takes out, washing, drying.The present invention is significantly reduced with product leakage current, and since forming current density doubles, the chemical conversion time reduces half, and seven sections of chemical conversions are changed to five sections of chemical conversions, and production efficiency is enhanced about more than once.
Description
Technical field
The present invention relates to the chemical synthesizing method for reducing capacitor anode foils leakage current, it is particularly suitable for reducing mesohigh aluminium electricity
The chemical synthesizing method of electrolysis condenser anode foils leakage current.
Background technique
The manufacture of electrode foil for aluminum electrolytic capacitors need to form one layer of fine and close oxidation film in aluminium foil surface, as capacitor
The working media of device.For its method frequently with formation processing method, so-called chemical conversion treatment is with chemistry or electrochemical method processing gold
Metal surface, obtains the coating of metallic compound, and purpose has improvement corrosion resistance, painting adhesion, metal coloring and chemical grinding
The effects of.
Chemical conversion system mainly has boric acid to form liquid system at present, phosphoric acid forms liquid system, adipic acid forms liquid system.Institute's body
System haves the defects that different degrees of.
CN201310178213.9 discloses a kind of formation processing method for reducing medium-high pressure chemical foil leakage current, feature
Be, comprising the following steps: A, excessive erosion of learning from else's experience, purity be 99.99% aluminium foil, aluminium foil is soaked into 8-12 in 95 DEG C of water
Minute is placed in mass percent 0.1-8% hexanedioic acid saline solution, in 70-95 DEG C, current density 20mA/cm2, voltage
Under conditions of 200V, level-one is melted into 8-12 minutes, takes out first wash；B, the aluminium foil after primary washing is placed in quality hundred
In hexanedioic acid saline solution point than 0.1-6%, 70-95 DEG C, current density 20mA/cm2, voltage be 430V condition
Under, second level is melted into 8-12 minutes, takes out second wash；C, the aluminium foil after secondary washing is placed in mass percent 0.1-4%
Hexanedioic acid saline solution in, 70-95 DEG C, current density 20mA/cm2, voltage be 590V under conditions of, three-level is melted into 8-
12 minutes；D, the aluminium foil after being melted into three-level is placed in aqueous solution identical with three-level, in 70-95 DEG C, current density 20mA/
Under conditions of cm2, voltage are 620V, level Four is melted into 24-36 minutes, and high-temperature heat treatment 1-4 points of 400-500 DEG C are carried out after taking-up
Clock；E, the aluminium foil after high-temperature process is placed in the borax solution of mass percent 1-5%, under conditions of 85-95 DEG C, leaching
Stain 3-8 minutes, then be placed in the boric acid of mass percent 4-9% and the borax solution of 0.1-1%, 70-95 DEG C, electric current it is close
Under conditions of degree is 20mA/cm2, voltage is 620V, Pyatyi is melted into 8-12 minutes；F, the aluminium foil after being melted into Pyatyi is in quality hundred
Divide temperature in the phosphoric acid solution than 1-8% to be handled for 50-80 DEG C, then takes out and carry out third time washing；It G, will water three times
Aluminium foil after washing is placed in the boric acid of mass percent 4-9% and the borax solution of 0.1-1%, in 70-95 DEG C, current density
Under conditions of being 620V for 20mA/cm2, voltage, six grades chemical conversion 8-12 minutes, then take out, carry out 400-500 DEG C of high warm
Processing 1-4 minutes；H, by the aluminium foil after high-temperature process be placed in mass percent 4-9% boric acid and 0.1-1% borax it is water-soluble
In liquid, 70-95 DEG C, current density 20mA/cm2, voltage be 620V under conditions of, seven grades are melted into 10 minutes, then take out
It being placed in mass percent 1-5% phosphate dihydrogen salt solution again, under the conditions of 70-95 DEG C, dipping takes out after 4-6 minutes, it washes,
Drying.
Chinese patent application CN201010158549.5 discloses the five of a kind of medium-high voltage aluminum electrolytic capacitor electrode foil
Grade manufacturing method: aluminium foil is soaked 10 minutes in 95 DEG C of water, in the aqueous solution for taking out the citrate for being placed in citric acid sum,
Under conditions of certain, level-one is melted into 8-15 minutes；Take out washing；It is placed in the azelaic acid of 0.1-5% and the azelate of 0.1-5%
Aqueous solution in, under certain condition, two/tri-/level Four be melted into 10 minutes；It is placed in the azelaic acid of 0.1-3% and the nonyl of 0.1-3%
In the aqueous solution of diacid salt, under certain conditions, Pyatyi is melted into 10 minutes；500 DEG C of high-temperature heat treatment 3-4 is carried out after taking-up
Minute；It is placed in the aqueous solution for being same as Pyatyi chemical conversion, under certain conditions, is melted into 10 minutes again；Then in the phosphoric acid of 1-8%
Temperature is handled in solution for 50-80 DEG C；It is placed in the aqueous solution for being same as Pyatyi chemical conversion again, under certain conditions, chemical conversion
10 minutes；It takes out, drying.
It is not difficult to find out that chemical synthesizing method disclosed in Chinese patent application CN201310178213.9 includes seven grades of chemical conversions, technique
Complexity, and time-consuming, production efficiency is low.Although Chinese patent application CN201010158549.5 discloses more simplified work
Skill only includes 5 grades of chemical conversions, but the electrode foil current-leakage amount of this method preparation is larger, and still unresolved production efficiency is low
The problem of, process flow time-consuming is still longer.
Summary of the invention
The purpose of the present invention is to overcome the above shortcomings, and it is small to provide a kind of product leakage current, extends capacitor and uses
Service life, the chemical synthesizing method of the reduction medium-high pressure chemical foil leakage current of high production efficiency.
The purpose of the present invention is achieved through the following technical solutions.
The present invention relates to a kind of chemical synthesizing methods for reducing medium-high pressure chemical foil leakage current, comprising the following steps:
A, aluminium foil that learn from else's experience excessive erosion, that purity is 99.99%, soaks 4-6 minutes postpositions for aluminium foil in 80-90 DEG C of water
In mass percent 0.1-4% azelate aqueous solution, in 75-85 DEG C, current density 40mA/cm2, voltage be 150V
Under the conditions of, level-one is melted into 4-6 minutes, takes out first wash；
B, the aluminium foil after primary washing is placed in the azelate aqueous solution of mass percent 0.1-3%, in 75-85
DEG C, current density 40mA/cm2, voltage be 310V under conditions of, second level be melted into 4-6 minute, taking-up second wash；
C, the aluminium foil after secondary washing is placed in the azelate aqueous solution of mass percent 0.1-2%, in 75-85
DEG C, current density 40mA/cm2, voltage be 450V under conditions of, three-level be melted into 4-6 minutes；
D, the aluminium foil after being melted into three-level is placed in the 3 of 0.5-1%, in 5- dihydroxy-benzoic acid aqueous solution, in room temperature condition
Under, impregnate 1-3 minutes, 550-600 DEG C progress high-temperature heat treatment 1-3 minutes；
E, the aluminium foil after high-temperature heat treatment is placed in the boric acid of mass percent 1-3% and the strontium phosphate water of 0.1-0.5%
In solution, in 75-85 DEG C, current density 40mA/cm2, voltage be 580V under conditions of, level Four be melted into 4-6 minutes, then take
Out, high-temperature heat treatment 1-2 minutes of 550-600 DEG C are carried out；
F, the aluminium foil after high-temperature heat treatment is placed in the strontium phosphate aqueous solution of mass percent 0.1-0.5%, in 75-85
DEG C, current density 40mA/cm2, voltage be 650V under conditions of, Pyatyi be melted into 4-6 minutes, then take out and be placed in quality hundred again
Divide than in 1-3% phosphoric acid solution, under the conditions of 30-50 DEG C, dipping takes out after 2-3 minutes, washes, drying.
In chemical synthesizing method of the present invention, wherein the azelate is ammonium azelate, azelaic acid sodium or azelaic acid
Potassium.It is preferred that ammonium azelate or azelaic acid sodium.More preferable azelaic acid sodium.
As a preferred implementation manner, the present invention relates to it is a kind of reduce low-pressure chemical synthesis foil leakage current chemical synthesizing method,
The following steps are included:
A, aluminium foil that learn from else's experience excessive erosion, that purity is 99.99%, aluminium foil is soaked in 85 DEG C of water and is placed in matter after five minutes
It measures in 0.4% azelaic acid sodium water solution of percentage, in 78 DEG C, current density 40mA/cm2, voltage be 150V under conditions of, one
Grade chemical conversion 5 minutes, takes out first wash.
B, the aluminium foil after primary washing is placed in the azelaic acid sodium water solution of mass percent 1.5%, in 82 DEG C, electric current
Density is 40mA/cm2, voltage be 310V under conditions of, second level be melted into 4 minutes, take out second wash.
C, the aluminium foil after secondary washing is placed in the azelaic acid sodium water solution of mass percent 0.8%, in 80 DEG C, electric current
Density is 40mA/cm2, voltage be 450V under conditions of, three-level be melted into 5 minutes.
D, the aluminium foil after being melted into three-level is placed in the 3 of 0.7%, in 5- dihydroxy-benzoic acid aqueous solution, at room temperature,
Dipping 2 minutes, 580 DEG C progress high-temperature heat treatment 2 minutes.
E, the aluminium foil after high-temperature heat treatment is placed in the boric acid of mass percent 2% and 0.3% strontium phosphate aqueous solution,
In 77 DEG C, current density 40mA/cm2, voltage be 580V under conditions of, level Four be melted into 4 minutes, then take out, carry out 570 DEG C
High-temperature heat treatment 1 minute.
F, the aluminium foil after high-temperature heat treatment is placed in the strontium phosphate aqueous solution of mass percent 0.4%, in 78 DEG C, electric current
Density is 40mA/cm2, voltage be 650V under conditions of, Pyatyi be melted into 5 minutes, then take out and be placed in mass percent 1.5% again
In phosphoric acid solution, under the conditions of 42 DEG C, dipping takes out after 2 minutes, washes, drying.
In the method for the invention, it is found surprisingly that, 3,5- dihydroxy-benzoic acid solution dipping is introduced after three-level chemical conversion
Step, the specific chemical solutions of chemical conversion at different levels screening (one to three-level is azelate, and level Four is boric acid+strontium phosphate mixed solution,
Pyatyi is strontium phosphate), and cooperate specific current density and voltage conditions, the electric leakage flow rate of obtained product in each chemical conversion treatment
It substantially reduces, and the shortening due to being melted into the time, the production efficiency of anode foils greatly improves.
Specific embodiment
In order to deepen the understanding of the present invention, the present invention will be described in further detail with reference to the examples below, the embodiment
For explaining only the invention, it is not intended to limit the scope of the present invention..
Embodiment 1
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.99%, aluminium foil is soaked in 85 DEG C of water and is placed in quality after five minutes
In 0.4% azelaic acid sodium water solution of percentage, in 78 DEG C, current density 40mA/cm2, voltage be 150V under conditions of, level-one
First wash is taken out in chemical conversion 5 minutes.The azelaic acid sodium that aluminium foil after primary washing is placed in mass percent 1.5% is water-soluble
In liquid, in 82 DEG C, current density 40mA/cm2, voltage be 310V under conditions of, second level be melted into 4 minutes, take out second of water
It washes.Aluminium foil after secondary washing is placed in the azelaic acid sodium water solution of mass percent 0.8%, is in 80 DEG C, current density
40mA/cm2, voltage be 450V under conditions of, three-level be melted into 5 minutes.Aluminium foil after three-level is melted into is placed in 0.7% 3,5- bis-
In hydroxybenzoic acid aqueous solution, at room temperature, impregnate 2 minutes, 580 DEG C progress high-temperature heat treatment 2 minutes.Height is warmed
Treated, and aluminium foil is placed in the boric acid of mass percent 2% and 0.3% strontium phosphate aqueous solution, is in 77 DEG C, current density
40mA/cm2, under conditions of voltage is 580V, level Four is melted into 4 minutes, is then taken out, and is carried out 570 DEG C of high-temperature heat treatment 1 and is divided
Clock.Aluminium foil after high-temperature heat treatment is placed in the strontium phosphate aqueous solution of mass percent 0.4%, is in 78 DEG C, current density
40mA/cm2, under conditions of voltage is 650V, Pyatyi is melted into 5 minutes, then takes out that be placed in 1.5% phosphoric acid of mass percent again molten
In liquid, under the conditions of 42 DEG C, dipping takes out after 2 minutes, washes, drying.
Embodiment 2
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.99%, aluminium foil is soaked in 88 DEG C of water and is placed in quality after five minutes
In 1.5% azelaic acid sodium water solution of percentage, in 77 DEG C, current density 40mA/cm2, voltage be 150V under conditions of, level-one
First wash is taken out in chemical conversion 4 minutes；The azelaic acid sodium that aluminium foil after primary washing is placed in mass percent 1.8% is water-soluble
In liquid, in 83 DEG C, current density 40mA/cm2, voltage be 310V under conditions of, second level be melted into 6 minutes, take out second of water
It washes；Aluminium foil after secondary washing is placed in the azelaic acid sodium water solution of mass percent 0.8%, is in 77 DEG C, current density
40mA/cm2, voltage be 450V under conditions of, three-level be melted into 6 minutes；Aluminium foil after three-level is melted into is placed in 0.9% 3,5- bis-
In hydroxybenzoic acid aqueous solution, at room temperature, impregnate 2 minutes, 580 DEG C progress high-temperature heat treatment 2 minutes；Height is warmed
Treated, and aluminium foil is placed in the boric acid of mass percent 1.8% and 0.4% strontium phosphate aqueous solution, in 81 DEG C, current density
For 40mA/cm2, under conditions of voltage is 580V, level Four is melted into 5 minutes, is then taken out, and is carried out 570 DEG C of high-temperature heat treatment 1 and is divided
Clock；Aluminium foil after high-temperature heat treatment is placed in the strontium phosphate aqueous solution of mass percent 0.4%, is in 77 DEG C, current density
40mA/cm2, under conditions of voltage is 650V, Pyatyi is melted into 4 minutes, then takes out that be placed in 2.5% phosphoric acid of mass percent again molten
In liquid, under the conditions of 48 DEG C, dipping takes out after 2 minutes, washes, drying.
Embodiment 3
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.99%, aluminium foil is soaked 6 minutes in 82 DEG C of water and is placed on quality
In 2% azelaic acid sodium water solution of percentage, in 80 DEG C, current density 40mA/cm2, voltage be 150V under conditions of, level-one
At 4 minutes, first wash is taken out；Aluminium foil after primary washing is placed in the azelaic acid sodium water solution of mass percent 1.2%
In, in 81 DEG C, current density 40mA/cm2, voltage be 310V under conditions of, second level be melted into 4 minutes, take out second wash；
Aluminium foil after secondary washing is placed in the azelaic acid sodium water solution of mass percent 1.3%, is in 80 DEG C, current density
40mA/cm2, voltage be 450V under conditions of, three-level be melted into 4 minutes；Aluminium foil after three-level is melted into is placed in 0.7% 3,5- bis-
In hydroxybenzoic acid aqueous solution, at room temperature, impregnate 2 minutes, 580 DEG C progress high-temperature heat treatment 3 minutes；Height is warmed
Treated, and aluminium foil is placed in the boric acid of mass percent 2.2% and 0.3% strontium phosphate aqueous solution, in 77 DEG C, current density
For 40mA/cm2, under conditions of voltage is 580V, level Four is melted into 4 minutes, is then taken out, and is carried out 580 DEG C of high-temperature heat treatment 1 and is divided
Clock；Aluminium foil after high-temperature heat treatment is placed in the strontium phosphate aqueous solution of mass percent 0.25%, is in 82 DEG C, current density
40mA/cm2, under conditions of voltage is 650V, Pyatyi is melted into 5 minutes, then takes out that be placed in 1.9% phosphoric acid of mass percent again molten
In liquid, under the conditions of 42 DEG C, dipping takes out after 2 minutes, washes, drying.
Embodiment 4
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.99%, aluminium foil is soaked 4 minutes in 87 DEG C of water and is placed on quality
In 0.9% azelaic acid sodium water solution of percentage, in 83 DEG C, current density 40mA/cm2, voltage be 150V under conditions of, level-one
First wash is taken out in chemical conversion 5 minutes；The azelaic acid sodium that aluminium foil after primary washing is placed in mass percent 2.5% is water-soluble
In liquid, in 79 DEG C, current density 40mA/cm2, voltage be 310V under conditions of, second level be melted into 6 minutes, take out second of water
It washes；Aluminium foil after secondary washing is placed in the azelaic acid sodium water solution of mass percent 1.8%, is in 82 DEG C, current density
40mA/cm2, voltage be 450V under conditions of, three-level be melted into 5 minutes；Aluminium foil after three-level is melted into is placed in 0.6% 3,5- bis-
In hydroxybenzoic acid aqueous solution, at room temperature, impregnate 2 minutes, 570 DEG C progress high-temperature heat treatment 2 minutes；Height is warmed
Treated, and aluminium foil is placed in the boric acid of mass percent 2.7% and 0.2% strontium phosphate aqueous solution, in 83 DEG C, current density
For 40mA/cm2, under conditions of voltage is 580V, level Four is melted into 6 minutes, is then taken out, and is carried out 590 DEG C of high-temperature heat treatment 2 and is divided
Clock；Aluminium foil after high-temperature heat treatment is placed in the strontium phosphate aqueous solution of mass percent 0.3%, is in 79 DEG C, current density
40mA/cm2, under conditions of voltage is 650V, Pyatyi is melted into 4 minutes, then takes out that be placed in 1.6% phosphoric acid of mass percent again molten
In liquid, under the conditions of 38 DEG C, dipping takes out after 2 minutes, washes, drying.
Comparative example 1
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.99%, impregnates 5 minutes, taking-up is placed in 90 DEG C of pure water
0.1% citric acid and 0.1% citrate aqueous solution in, 70 DEG C, current density be 20mA/ (cm) 2, voltage 140V
Under conditions of, level-one is melted into 8 minutes；It is rinsed with water after taking-up；It is placed in 0.1% azelaic acid and 0.1% azelate again
In aqueous solution, under conditions of 70 DEG C, current density are 20mA/ (cm) 2, voltage is 280V, second level is melted into 8 minutes；It is placed in again
0.1% azelaic acid and 0.1% azelate aqueous solution in, 70 DEG C, current density are 20mA/ (cm) 2, voltage is
Under conditions of 450V, three-level is melted into 8 minutes；It is placed in the aqueous solution of 0.1% azelaic acid and 0.1% azelate again,
70 DEG C, current density be 20mA/ (cm) 2, under conditions of voltage is 580V, level Four is melted into 8 minutes；It is placed in 0.1% nonyl two again
In the sour aqueous solution with 0.1% azelate, under conditions of 70 DEG C, current density are 20mA/ (cm) 2, voltage is 620V,
Pyatyi is melted into 8 minutes；Aluminium foil after Pyatyi is melted into takes out from electrolytic bath, carries out high-temperature heat treatment 3 minutes of 500 DEG C；
Be placed in the aqueous solution of 0.1% azelaic acid and 0.1% azelate again, 70 DEG C, current density be 20mA/ (cm) 2, electricity
Under conditions of pressure is 620V, it is melted into 8 minutes；Then temperature is handled in 1% phosphoric acid solution for 50 DEG C；It is placed in again
0.1% azelaic acid and 0.1% azelate aqueous solution in, 70 DEG C, current density are 20mA/ (cm) 2, voltage is
Under conditions of 620V, it is melted into 8 minutes；It finally takes out, dries.
Comparative example 2
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.99%, aluminium foil is soaked in 95 DEG C of water and is placed in quality after five minutes
In 8% hexanedioic acid saline solution of percentage, in 95 DEG C, current density 20mA/cm2, voltage be 200V under conditions of, level-one
At 10 minutes, first wash is taken out；Aluminium foil after primary washing is placed in the hexanedioic acid saline solution of mass percent 6%
In, in 85 DEG C, current density 20mA/cm2, voltage be 430V under conditions of, second level be melted into 10 minutes, take out second of water
It washes；Aluminium foil after secondary washing is placed in the hexanedioic acid saline solution of mass percent 4%, is in 85 DEG C, current density
20mA/cm2, voltage be 590V under conditions of, three-level be melted into 10 minutes；Aluminium foil after three-level is melted into is placed in identical with three-level
In aqueous solution, in 85 DEG C, current density 20mA/cm2, voltage be 620V under conditions of, level Four be melted into 30 minutes, take out it is laggard
The high-temperature heat treatment that 500 DEG C of row 3 minutes；Aluminium foil after high-temperature process is placed in the borax solution of mass percent 5%,
It under conditions of 85 DEG C, impregnates 3 minutes, then be placed in the boric acid of mass percent 9% and 1% borax solution, in 85 DEG C, electricity
Current density is 20mA/cm2, voltage be 620V under conditions of, Pyatyi be melted into 10 minutes；Aluminium foil after Pyatyi is melted into is in quality hundred
Divide temperature in the phosphoric acid solution than 8% to be handled for 80 DEG C, then takes out and carry out third time washing；By the aluminium after washing three times
Foil is placed in the boric acid of mass percent 9% and 1% borax solution, in 85 DEG C, current density 20mA/cm2, voltage be
Under conditions of 620V, six grades are melted into 10 minutes, then take out, and carry out high-temperature heat treatment 3 minutes of 500 DEG C；After high-temperature process
Aluminium foil be placed in the boric acid of mass percent 9% and 1% borax solution, in 85 DEG C, current density 20mA/cm2, electricity
Under conditions of pressure is 620V, seven grades are melted into 10 minutes, are then taken out and are placed in 5% phosphate dihydrogen salt solution of mass percent again,
Under the conditions of 95 DEG C, dipping takes out after five minutes, washes, drying.
By electrode foil that 1-5 of the embodiment of the present invention is obtained compared with the electrode foil that comparative example 1-2 is obtained carries out performance, as a result
It is as in the table below:
* the sum of dip time, chemical conversion time, heat treatment time
* efficiency improves=compares duration/handling duration -1
Said determination result is not difficult to find out that the production efficiency of the method for the present invention greatly improves.In addition, the method for the present invention obtains
The magnitude of leakage current of electrode foil be far smaller than comparative example method, 1 method of embodiment obtains the magnitude of leakage current of electrode foil as minimum, is
Most preferred method.Secondly, the obtained electrode foil of the method for the present invention capacity after storage 60 days is substantially unchanged, and control methods
The capacity of obtained electrode foil then decreases.
Although detailed description has been made to the present invention, and some specific examples are listed, to those skilled in the art
For member, as long as it does not depart from the spirit of the invention, and the various adjustment done to this method are regarded as being included in model of the invention
In enclosing.
Claims (8)
1. a kind of chemical synthesizing method for reducing medium-high pressure chemical foil leakage current, which comprises the following steps:
A, aluminium foil that learn from else's experience excessive erosion, that purity is 99.99%, aluminium foil is soaked 4-6 minutes in 80-90 DEG C of water and is placed on matter
It measures in percentage 0.1-4% azelate aqueous solution, in 75-85 DEG C, current density 40mA/cm2, voltage be 150V condition
Under, level-one is melted into 4-6 minutes, takes out first wash；
B, the aluminium foil after primary washing is placed in the azelate aqueous solution of mass percent 0.1-3%, in 75-85 DEG C, electricity
Current density is 40mA/cm2, voltage be 310V under conditions of, second level be melted into 4-6 minute, taking-up second wash；
C, the aluminium foil after secondary washing is placed in the azelate aqueous solution of mass percent 0.1-2%, in 75-85 DEG C, electricity
Current density is 40mA/cm2, voltage be 450V under conditions of, three-level be melted into 4-6 minutes；
D, the aluminium foil after being melted into three-level is placed in the 3 of 0.5-1%, in 5- dihydroxy-benzoic acid aqueous solution, at room temperature, leaching
Stain 1-3 minutes, 550-600 DEG C progress high-temperature heat treatment 1-3 minutes；
E, the aluminium foil after high-temperature heat treatment is placed in the boric acid of mass percent 1-3% and the strontium phosphate aqueous solution of 0.1-0.5%
In, in 75-85 DEG C, current density 40mA/cm2, voltage be 580V under conditions of, level Four be melted into 4-6 minutes, then take out,
Carry out high-temperature heat treatment 1-2 minutes of 550-600 DEG C；
F, the aluminium foil after high-temperature heat treatment is placed in the strontium phosphate aqueous solution of mass percent 0.1-0.5%, 75-85 DEG C,
Current density is 40mA/cm2, voltage be 650V under conditions of, Pyatyi be melted into 4-6 minutes, then take out and be placed in quality percentage again
Than in 1-3% phosphoric acid solution, under the conditions of 30-50 DEG C, dipping takes out after 2-3 minutes, wash, drying.
2. chemical synthesizing method according to claim 1, which is characterized in that in step, excessive erosion of learning from else's experience, purity be
Aluminium foil is soaked in 85 DEG C of water and is placed in 0.4% azelate aqueous solution of mass percent after five minutes by 99.99% aluminium foil,
In 78 DEG C, current density 40mA/cm2, voltage be 150V under conditions of, level-one be melted into 5 minutes, take out first wash.
3. chemical synthesizing method according to claim 1, which is characterized in that in stepb, the aluminium foil after primary washing is placed in
In the azelate aqueous solution of mass percent 1.5%, in 82 DEG C, current density 40mA/cm2, voltage be 310V condition
Under, second level is melted into 4 minutes, takes out second wash.
4. chemical synthesizing method according to claim 1, which is characterized in that in step C, the aluminium foil after secondary washing is placed in
In the azelate aqueous solution of mass percent 0.8%, in 80 DEG C, current density 40mA/cm2, voltage be 450V condition
Under, three-level is melted into 5 minutes.
5. chemical synthesizing method according to claim 1, which is characterized in that in step D, the aluminium foil after three-level is melted into is placed in
In 0.7% 3,5- dihydroxy-benzoic acid aqueous solution, at room temperature, impregnate 2 minutes, in 580 DEG C of progress high-temperature heat treatments 2
Minute.
6. chemical synthesizing method according to claim 1, which is characterized in that in step E, the aluminium foil after high-temperature heat treatment is set
In the boric acid of mass percent 2% and 0.3% strontium phosphate aqueous solution, in 77 DEG C, current density 40mA/cm2, voltage be
Under conditions of 580V, level Four is melted into 4 minutes, is then taken out, and high-temperature heat treatment 1 minute of 570 DEG C is carried out.
7. chemical synthesizing method according to claim 1, which is characterized in that in step F, the aluminium foil after high-temperature heat treatment is set
In the strontium phosphate aqueous solution of mass percent 0.4%, in 78 DEG C, current density 40mA/cm2, voltage be 650V condition
Under, Pyatyi is melted into 5 minutes, is then taken out and is placed in 1.5% phosphoric acid solution of mass percent again, under the conditions of 42 DEG C, impregnates 2 points
It takes out, washes after clock, drying.
8. chemical synthesizing method according to claim 1, it is characterised in that: the azelate is ammonium azelate, azelaic acid sodium
Or azelaic acid potassium.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3872579A (en) * | 1973-04-11 | 1975-03-25 | Cornell Dubilier Electric | Method of making electrolytic capacitors |
| CN101826397A (en) * | 2010-04-27 | 2010-09-08 | 四川中雅科技有限公司 | Five-stage manufacturing method of electrode foil for medium-high voltage aluminium electrolytic capacitor |
| CN102709059A (en) * | 2012-06-09 | 2012-10-03 | 永济粟海铝业有限公司 | Formation method for anode foil of intermediate-voltage aluminum electrolytic capacitor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3872579A (en) * | 1973-04-11 | 1975-03-25 | Cornell Dubilier Electric | Method of making electrolytic capacitors |
| CN101826397A (en) * | 2010-04-27 | 2010-09-08 | 四川中雅科技有限公司 | Five-stage manufacturing method of electrode foil for medium-high voltage aluminium electrolytic capacitor |
| CN102709059A (en) * | 2012-06-09 | 2012-10-03 | 永济粟海铝业有限公司 | Formation method for anode foil of intermediate-voltage aluminum electrolytic capacitor |
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