CN105702465A - Method for manufacturing electrode foil of UPS - Google Patents
Method for manufacturing electrode foil of UPS Download PDFInfo
- Publication number
- CN105702465A CN105702465A CN201610030428.XA CN201610030428A CN105702465A CN 105702465 A CN105702465 A CN 105702465A CN 201610030428 A CN201610030428 A CN 201610030428A CN 105702465 A CN105702465 A CN 105702465A
- Authority
- CN
- China
- Prior art keywords
- aqueous solution
- aluminum foil
- electrode foil
- mixed aqueous
- ammonium adipate
- 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
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- 239000011888 foil Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000007864 aqueous solution Substances 0.000 claims abstract description 33
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 29
- 235000019253 formic acid Nutrition 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 19
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001741 Ammonium adipate Substances 0.000 claims abstract description 17
- 235000019293 ammonium adipate Nutrition 0.000 claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000012805 post-processing Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 19
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000005030 aluminium foil Substances 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 9
- 238000007654 immersion Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 4
- 235000011149 sulphuric acid Nutrition 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 8
- -1 sulfate radical ions Chemical class 0.000 abstract description 3
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000007669 thermal treatment Methods 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 238000000866 electrolytic etching Methods 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 210000000981 epithelium Anatomy 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000002699 waste material Substances 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
- 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)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- ing And Chemical Polishing (AREA)
Abstract
The invention discloses a method for manufacturing electrode foil of a UPS. The method comprise steps of: immersing aluminum foil in sodium hydroxide solution; placing the aluminum foil in mixed aqueous solution and powering and corroding the aluminum foil; placing the aluminum foil in mixed solution containing glycollic acid and formic acid to perform postprocessing cleaning; immersing the aluminum foil in pure water at 20 degrees centigrade; placing the aluminum foil in a baking oven and performing thermal treatment at 450 degrees centigrade; applying 8V voltage to the aluminum foil in ammonium adipate aqueous solution to perform formation treatment, and drying the aluminum foil. The method has advantages of effectively controlling the content of chloride ions of the electrode foil under 5ppm and the content of sulfate radical ions under 0.5ppm, greatly reducing the leakage current of the electrode foil, prolonging the service life, forming a pure oxide skin film, and increasing capacity.
Description
Technical field
The present invention relates to the manufacture method of a kind of ups power electrode foil。
Background technology
In general, low-voltage electrolytic capacitor aluminum electric pole foil, in the aqueous solution through mixing containing hydrochloric acid, sulphuric acid, nitric acid and phosphoric acid etc., after carrying out chemistry or electrochemical corrosion, a large amount of chloride ion are adhered in paper tinsel face, the foreign ions such as sulfate ion, follow-up, need the foreign ion adopting certain cleaning solution to remove attachment。And after a washing process, eliminate the foreign ion of the pre-treatment flow process of the former paper tinsel surface attachment of aluminum, corrosion process in a large number, therefore in postorder flow process, paper tinsel face hydration epithelium and heat-treatment oxidation epithelium are easily formed, the static capacity of Waste Acid From Hua Cheng Foil can be effectively improved, reduce electrode foil current-leakage simultaneously, promote its service life。
The chloride ion of paper tinsel face attachment after conventional clean electrolytic etching, the method for the foreign ions such as sulfate ion is, the method soaked in the inorganic aqueous acid such as nitric acid or sulphuric acid。
Summary of the invention
It is an object of the invention to improve paper tinsel face cleaning way, paper tinsel face foreign ion clearance is substantially improved, while improving electrode foil capacity, electrode foil current-leakage is greatly reduced, promote its service life, to adapt to ups power uninterrupted discharge and recharge in 24 hours and the requirement of long life。
The purpose of the present invention is achieved through the following technical solutions: the manufacture method of a kind of ups power electrode foil, and step is as follows,
A, purity are that the 97 μ m thick aluminium foils of 99.99% soak 1 minute at the sodium hydroxide solution of 0.2mol/L, reaction temperature 20 ~ 60 DEG C；Being subsequently placed in mixed aqueous solution and once add galvano-cautery, powering up frequency is 20 ~ 50Hz, and reaction temperature is 30 ~ 50 DEG C, and the response time is 30s；Being placed in chemical attack in mixed aqueous solution again, reaction temperature is 50 ~ 70 DEG C, and the response time is 1min30s；Then being placed in mixed aqueous solution to carry out secondary and add galvano-cautery, powering up frequency is 20 ~ 50Hz, and reaction temperature is 20 ~ 40 DEG C, and the response time is 2min20s；Being placed in mixed aqueous solution again to carry out three times and add galvano-cautery, powering up frequency is 20 ~ 50Hz, and reaction temperature is 20 ~ 40 DEG C, and the response time is 3min15s。
B, being placed in by aluminium foil in the mixed solution containing 4% ~ 12% glycolic and 0.8% ~ 1.6% formic acid and carry out post processing cleaning, post processing rinse bath liquid temp is 30 ~ 85 DEG C, response time 4min ~ 6min；
C, in 20 DEG C of pure water immersion treatment, soak time 8min ~ 12min；
D, aluminium foil being placed in baking oven, carry out heat treatment at 450 DEG C, heat treatment process carries out in inert gas shielding atmosphere simultaneously, processes time 20s ~ 60s；
E, at 60 ~ 80 DEG C, carry out chemical conversion treatment 2 ~ 4min containing the voltage applying 8V in the aqueous solution of the ammonium adipate of 3% ~ 10%；It is subsequently placed in 70 ~ 90 DEG C, carries out chemical conversion treatment 2 ~ 4min containing the voltage applying 27V in the aqueous solution of the ammonium adipate of 3% ~ 10%；It is placed in 70 ~ 90 DEG C again, carries out chemical conversion treatment 2 ~ 10min containing the voltage applying 34V in the aqueous solution of the ammonium adipate of 3% ~ 10%；Then it is placed in 30 ~ 60 DEG C, one or more mixed aqueous solution of phosphoric acid and ammonium adipate processes 2 ~ 10min；It is subsequently placed in baking oven, at 450 DEG C, carries out heat treatment, process time 20s ~ 60s；It is placed in 30 ~ 60 DEG C again, one or more mixed aqueous solution of phosphoric acid and ammonium adipate processes 2 ~ 10min；Then immersion treatment in 20 DEG C of pure water, soak time 8min ~ 12min it are placed in；Finally dry。
Preferably, the mixed aqueous solution that corrosive water solution is hydrochloric acid, sulphuric acid and phosphoric acid is powered up。
Preferably, post processing aqueous solution is 4% ~ 12% glycolic and the mixed solution of 0.8% ~ 1.6% formic acid。
Preferably, chemical conversion treatment aqueous solution is one or more mixed aqueous solution of phosphoric acid and ammonium adipate。
In sum, the invention have the advantages that and can effectively control electrode foil chloride ion content at below 5ppm, sulfate ion content, at below 0.5ppm, is greatly reduced electrode foil current-leakage, promotes service life；Concurrently forming pure oxide scale film, capacity raises to some extent。
Detailed description of the invention
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment is only used for explaining the present invention, is not intended that limiting the scope of the present invention。
Embodiment 1: glycolic concentration 4%, formic acid concn 1.0%, rinse liquid temperature 50 DEG C。
Embodiment 2: glycolic concentration 6%, formic acid concn 1.0%, rinse liquid temperature 50 DEG C。
Embodiment 3: glycolic concentration 8%, formic acid concn 1.0%, rinse liquid temperature 50 DEG C。
Embodiment 4: glycolic concentration 10%, formic acid concn 0.8%, rinse liquid temperature 50 DEG C。
Embodiment 5: glycolic concentration 10%, formic acid concn 1.0%, rinse liquid temperature 50 DEG C。
Embodiment 6: glycolic concentration 10%, formic acid concn 1.2%, rinse liquid temperature 50 DEG C。
Embodiment 7: glycolic concentration 10%, formic acid concn 1.4%, rinse liquid temperature 50 DEG C。
Embodiment 8: glycolic concentration 10%, formic acid concn 1.6%, rinse liquid temperature 50 DEG C。
Embodiment 9: glycolic concentration 12%, formic acid concn 1.0%, rinse liquid temperature 50 DEG C。
Embodiment 10: glycolic concentration 8%, formic acid concn 1.0%, rinse liquid temperature 30 DEG C。
Embodiment 11: glycolic concentration 8%, formic acid concn 1.0%, rinse liquid temperature 40 DEG C。
Embodiment 12: glycolic concentration 8%, formic acid concn 1.0%, rinse liquid temperature 60 DEG C。
Embodiment 13: glycolic concentration 8%, formic acid concn 1.0%, rinse liquid temperature 70 DEG C。
Embodiment 14: glycolic concentration 8%, formic acid concn 1.0%, rinse liquid temperature 80 DEG C。
Embodiment 15: glycolic concentration 8%, formic acid concn 1.0%, rinse liquid temperature 85 DEG C。
In embodiment 1,2,3,5,9 cleanout fluid, glycolic concentration compares:
Purity is that the 97 μ m thick aluminium foils of 99.99% are after carrying out multistage electrolytic etching, containing 4% ~ 12% glycolic, the solution of 1.0% formic acid cleans, solution temperature is 50 DEG C, then in pure water after immersion treatment, then the heat treatment of 450 DEG C has been carried out, finally at 85 DEG C, the voltage applying 20V in aqueous solution containing 6.0% ammonium adipate carries out chemical conversion treatment, tests static capacity。
It addition, cleaned on electrode foil surface after a washing process, take 100cm2Electrode foil, dissolves with 0.05mol/L sodium hydroxide, uses the chromatography of ions, measures chloride ion and sulfate ion content。
In embodiment 4,5,6,7,8 cleanout fluid, formic acid concn compares:
Purity is that the 97 μ m thick aluminium foils of 99.99% are after carrying out multistage electrolytic etching, containing 10% glycolic, the solution of 0.8% ~ 1.6% formic acid cleans, solution temperature is 50 DEG C, then in pure water after immersion treatment, then the heat treatment of 450 DEG C has been carried out, finally at 85 DEG C, the voltage applying 20V in aqueous solution containing 6.0% ammonium adipate carries out chemical conversion treatment, tests static capacity。
Embodiment 3,10,11,12,13,14,15 rinse liquid temperature compares:
Purity is that the 97 μ m thick aluminium foils of 99.99% are after carrying out multistage electrolytic etching, containing 8% glycolic, the solution of 1.0% formic acid cleans, solution temperature is 30 DEG C ~ 85 DEG C, then in pure water after immersion treatment, then the heat treatment of 450 DEG C has been carried out, finally at 85 DEG C, the voltage applying 20V in aqueous solution containing 6.0% ammonium adipate carries out chemical conversion treatment, tests static capacity。
Conventional case:
Purity is that the 97 μ m thick aluminium foils of 99.99% are after carrying out multistage electrolytic etching, solution containing 0.75% nitric acid cleans, solution temperature is 50 DEG C, then in pure water after immersion treatment, carry out the heat treatment of 450 DEG C again, last at 85 DEG C, the voltage applying 20V in the aqueous solution containing 6.0% ammonium adipate carries out chemical conversion treatment, tests static capacity。
Above-mentioned comparison draws data such as table 1:
In cleanout fluid, glycolic concentration compares:
As can be seen from Table 1, when fixing formic acid concn is 1.0wt% and solution temperature is 50 DEG C, when glycolic concentration is 8wt%, 10wt% and 12wt%, chloride ion and sulfate ion content are relatively low, but when glycolic concentration is 12wt%, electrode foil capacity occurs in that decay。
In cleanout fluid, formic acid concn compares:
As can be seen from Table 1, when fixing glycolic concentration is 10wt% and solution temperature is 50 DEG C, when formic acid concn is 1.2wt%, 1.4wt% and 1.6wt%, cleaning performance is best, chloride ion and sulfate ion content are relatively low, but when formic acid concn is 1.6wt%, electrode foil capacity occurs in that decay。
Rinse liquid temperature compares:
As it can be seen from table 1 be 8wt% in fixing glycolic concentration, when formic acid concn is 1.0wt%, when solution temperature is 70 DEG C, 80 DEG C and 85 DEG C, cleaning performance is best, and chloride ion and sulfate ion content are low, but when solution temperature is 85 DEG C, electrode foil capacity occurs in that decays by a relatively large margin。
Claims (4)
1. the manufacture method of a ups power electrode foil, it is characterised in that: step is as follows,
A, purity are that the 97 μ m thick aluminium foils of 99.99% soak 1 minute at the sodium hydroxide solution of 0.2mol/L, reaction temperature 20 ~ 60 DEG C；Being subsequently placed in mixed aqueous solution and once add galvano-cautery, powering up frequency is 20 ~ 50Hz, and reaction temperature is 30 ~ 50 DEG C, and the response time is 30s；Being placed in chemical attack in mixed aqueous solution again, reaction temperature is 50 ~ 70 DEG C, and the response time is 1min30s；Then being placed in mixed aqueous solution to carry out secondary and add galvano-cautery, powering up frequency is 20 ~ 50Hz, and reaction temperature is 20 ~ 40 DEG C, and the response time is 2min20s；Being placed in mixed aqueous solution again to carry out three times and add galvano-cautery, powering up frequency is 20 ~ 50Hz, and reaction temperature is 20 ~ 40 DEG C, and the response time is 3min15s；
B, being placed in by aluminium foil in the mixed solution containing 4% ~ 12% glycolic and 0.8% ~ 1.6% formic acid and carry out post processing cleaning, post processing rinse bath liquid temp is 30 ~ 85 DEG C, response time 4min ~ 6min；
C, in 20 DEG C of pure water immersion treatment, soak time 8min ~ 12min；
D, aluminium foil being placed in baking oven, carry out heat treatment at 450 DEG C, heat treatment process carries out in inert gas shielding atmosphere simultaneously, processes time 20s ~ 60s；
E, at 60 ~ 80 DEG C, carry out chemical conversion treatment 2 ~ 4min containing the voltage applying 8V in the aqueous solution of the ammonium adipate of 3% ~ 10%；It is subsequently placed in 70 ~ 90 DEG C, carries out chemical conversion treatment 2 ~ 4min containing the voltage applying 27V in the aqueous solution of the ammonium adipate of 3% ~ 10%；It is placed in 70 ~ 90 DEG C again, carries out chemical conversion treatment 2 ~ 10min containing the voltage applying 34V in the aqueous solution of the ammonium adipate of 3% ~ 10%；Then it is placed in 30 ~ 60 DEG C, one or more mixed aqueous solution of phosphoric acid and ammonium adipate processes 2 ~ 10min；It is subsequently placed in baking oven, at 450 DEG C, carries out heat treatment, process time 20s ~ 60s；It is placed in 30 ~ 60 DEG C again, one or more mixed aqueous solution of phosphoric acid and ammonium adipate processes 2 ~ 10min；Then immersion treatment in 20 DEG C of pure water, soak time 8min ~ 12min it are placed in；Finally dry。
2. the manufacture method of a kind of ups power electrode foil according to claim 1, it is characterised in that: described in power up the mixed aqueous solution that corrosive water solution is hydrochloric acid, sulphuric acid and phosphoric acid。
3. the manufacture method of a kind of ups power electrode foil according to claim 1, it is characterised in that: described in add post processing aqueous solution be 4% ~ 12% glycolic and the mixed solution of 0.8% ~ 1.6% formic acid。
4. the manufacture method of a kind of ups power electrode foil according to claim 1, it is characterised in that: described chemical conversion treatment aqueous solution is one or more mixed aqueous solution of phosphoric acid and ammonium adipate。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610030428.XA CN105702465B (en) | 2016-01-18 | 2016-01-18 | A kind of manufacture method of ups power electrode foil |
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| CN201610030428.XA CN105702465B (en) | 2016-01-18 | 2016-01-18 | A kind of manufacture method of ups power electrode foil |
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| CN105702465A true CN105702465A (en) | 2016-06-22 |
| CN105702465B CN105702465B (en) | 2017-09-29 |
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| CN107452509A (en) * | 2017-06-27 | 2017-12-08 | 苏州菱慧电子科技有限公司 | A kind of production technology of aluminium electrolutic capacitor |
| CN109599269A (en) * | 2018-11-30 | 2019-04-09 | 南通海星电子股份有限公司 | The manufacturing method of surface mount electrode foil for aluminum electrolytic capacitors |
| CN109741954A (en) * | 2019-03-04 | 2019-05-10 | 益阳艾华富贤电子有限公司 | A kind of solid-state aluminum electrolytic capacitor preparation process using efficient chemical synthesizing method |
| CN110474058A (en) * | 2019-09-18 | 2019-11-19 | 南通海星电子股份有限公司 | A kind of preparation method of template cathodic oxygen reduction electro-catalysis Pt electrode |
| WO2019227903A1 (en) * | 2018-05-31 | 2019-12-05 | 南通海星电子股份有限公司 | Manufacturing method for middle-high voltage corrosion foil for aluminum electrolytic capacitor |
| CN111189818A (en) * | 2018-11-15 | 2020-05-22 | 东莞东阳光科研发有限公司 | Detection box for detecting residual chloride ions on surface of electrode foil as well as preparation method and application of detection box |
| CN111330535A (en) * | 2020-03-25 | 2020-06-26 | 南通海星电子股份有限公司 | Novel adsorption material for water treatment and preparation method thereof |
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| CN111189818A (en) * | 2018-11-15 | 2020-05-22 | 东莞东阳光科研发有限公司 | Detection box for detecting residual chloride ions on surface of electrode foil as well as preparation method and application of detection box |
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| CN109741954A (en) * | 2019-03-04 | 2019-05-10 | 益阳艾华富贤电子有限公司 | A kind of solid-state aluminum electrolytic capacitor preparation process using efficient chemical synthesizing method |
| CN109741954B (en) * | 2019-03-04 | 2020-11-06 | 益阳艾华富贤电子有限公司 | Solid-state aluminum electrolytic capacitor preparation process adopting efficient formation method |
| CN110474058A (en) * | 2019-09-18 | 2019-11-19 | 南通海星电子股份有限公司 | A kind of preparation method of template cathodic oxygen reduction electro-catalysis Pt electrode |
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