CN104078240A - Method for manufacturing anode foil of alternating current motor capacitor - Google Patents
Method for manufacturing anode foil of alternating current motor capacitor Download PDFInfo
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- CN104078240A CN104078240A CN201410319321.8A CN201410319321A CN104078240A CN 104078240 A CN104078240 A CN 104078240A CN 201410319321 A CN201410319321 A CN 201410319321A CN 104078240 A CN104078240 A CN 104078240A
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Abstract
The invention discloses a method for manufacturing anode foil of an alternating current motor capacitor. The method includes the steps of hydration processing, five-stage formation processing, high-temperature heat processing, depolarization processing, repairing formation processing, post-processing and drying processing, and is characterized in that the formation preprocessing step is additionally executed after the hydration processing step, the hydration processing step is that immersion processing is carried out with an ethanediol water solution, and the formation preprocessing step is that the corroded foil obtained after hydration processing is placed into a maleic acid solution for immersing processing. According to the method, hydration processing is carried out in the first stage of the anode oxide film forming working procedure with the ethanediol water solution, and the dielectric property of anode oxide film is improved; the corroded foil obtained after hydration processing is processed with the maleic acid to prevent the foil from being seriously corroded, and the water resisting property of the oxide film is finally achieved; formation is carried out with phosphoric acid and a saline solution of the phosphoric acid in first-stage formation processing and second-stage formation processing, and the specific volume is easily improved; meanwhile, due to the fact that phosphoric acid film is thin, the bending strength of the formed foil can be obviously improved.
Description
Technical field
The present invention relates to a kind of anode foil manufacturing method for alternating current motor capacitor, belong to electrolytic capacitor and manufacture field with being anodizing to paper tinsel.
Background technology
Corrosion process is to take electronic light paper tinsel as raw material, forms hole, thereby increase the surface area of negative electrode, anode light paper tinsel by electrochemical method etching electronic light paper tinsel surface, to improve it, than electric capacity, makes etched foil.
The preparation method of the anode foils of at present domestic existing many aluminium electrolytic capacitors, generally that etched foil is carried out to high temperature Pure water preparation, etched foil first generates one deck aqua oxidation film, again in inorganic acid or organic acid or mixed acid, seal adds certain formation voltage and changes into processing, after arriving fixed formation voltage, be impregnated in phosphoric acid solution, and carry out 450-550 ℃ of heat treatment of placing several minutes and carry out depolarising processing, the space and the be full of cracks that make to become in the oxide-film of leakage current reason expose, according to repeatedly repairing and change into, form desirable anodic oxide coating.
In conventional art, aluminium foil carries out hydration-treated in high temperature pure water, at aluminium foil surface, can form one deck hydroxide, when forming, this hydroxide can be converted into boehmite again, therefore wish to generate the most easily change into γ-AL2O3 take γ-diaspore as main hydroxide, in atmosphere, the temperature of hydration process is below 100 ℃, at this temperature, can not generate real γ-diaspore, but class boehmite.From microscope, can find out, class boehmite is divided into part and the outer fiber shape part that internal density is high, inner moisture few, approaches γ-diaspore, easily changes into γ-AL2O3 when forming, and outside moisture many, is difficult to change into γ-AL2O3 state.The features such as thereby the dielectric property of anode foils are poor, and leakage current is large, and hydration characteristic is poor.
While starting due to alternating current motor, electric current is larger, discharge and recharge very frequent, higher to the requirement of Waste Acid From Hua Cheng Foil, because leakage current in the prepared Waste Acid From Hua Cheng Foil of method of the prior art is large, can not meet in modern application the needs for alternating current motor capacitor.
Summary of the invention
The object of the invention is to for deficiency of the prior art, a kind of anode foil manufacturing method for alternating current motor capacitor is provided, the Waste Acid From Hua Cheng Foil making not only has good dielectric property, and warpage intensity is good especially.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of anode foil manufacturing method for alternating current motor capacitor, comprise that hydration-treated, Pyatyi change into processing, high-temperature heat treatment, depolarising and process, repair and change into processing, reprocessing and drying and processing, its innovative point is: after described hydration-treated step, increase and change into pre-treatment step;
Described hydration-treated step is for adopting glycol water to carry out impregnation process; Be specially pit as running through type, and etched foils more than average pore size 1.5 μ m to put into concentration be 0.1-30wt%, temperature is impregnation process 1-10min in the ethylene glycol solution of 60-100 ℃;
Describedly change into pre-treatment step for etched foil that hydration-treated is crossed, to put into concentration be 0.01-0.5wt%, temperature is to carry out impregnation process in the maleic acid solution of 70-95 ℃, and the time that impregnation process is set is 10s-5min.
Further, in described hydration-treated step ethylene glycol solution concentration be 0.5-30wt%.
Further, to change into the electrolyte that first and second grade in processing change into use be aqueous phosphatic to described Pyatyi.
Further, described one-level changes into process and is specially that to be placed in concentration be 0.01-0.3wt% by changing into pretreated etched foil, and temperature is the aqueous phosphatic of 60-90 ℃, and it is 10-30mA/cm that current density is set
2, voltage is 30% seal making alive, changes into and processes 5-20 minute.
Further, described secondary changes into process to be specially and through one-level, changes into the etched foil of processing to be placed in concentration be 0.01-0.1wt%, and in the phosphate solution of temperature 60-90 ℃, it is 10-30mA/cm that current density is set
2, the seal making alive that voltage is 60%, changes into and processes 5-20 minute.
Further, to change into the electrolyte that third and fourth and Pyatyi in processing change into be that concentration is that boric acid and the concentration of 1-12wt% is the mixed solution of 0.01-0.2wt% ammonium pentaborate to described Pyatyi.
Further, described the 3rd polarization is processed the etched foil being specially after two utmost point polarization are processed and is taken out washing 2 minutes; Be placed in again boric acid and 0.01-0.2wt% ammonium pentaborate mixed solution that concentration is 1-12wt%, set temperature 60-90 ℃, current density 10-30mA/cm
2, the seal making alive that voltage is 78%, changes into and processes 5-20 minute.
Further, described the 4th polarization is processed after the etched foil being specially after three utmost point polarization are processed takes out and is placed in boric acid and the 0.01-0.1wt% ammonium pentaborate mixed solution that concentration is 1-10wt%, set temperature 60-90 ℃, current density 10-30mA/cm again
2, the seal making alive that voltage is 90%, changes into and processes 5-20 minute.
Further, described the 5th polarization is processed after the etched foil being specially after four utmost point polarization are processed takes out and is placed in boric acid and the 0.01-0.06wt% ammonium pentaborate mixed solution that concentration is 1-10wt% again, solution temperature 60-90 ℃ is set, current density 10-30mA/cm
2, the seal making alive that voltage is 100%, changes into and processes 15-60 minute.
Further, described reprocessing is for being used phosphate solution to flood, and set temperature is 50-90 ℃, and the processing time is 1.5-4.5min; The concentration of described phosphate solution is 0.1-5wt%.
Beneficial effect of the present invention is as follows:
(1) at anode oxide film, form the leading portion of operation, the spent glycol aqueous solution carries out hydration-treated, aluminium foil surface generates one deck hydroxide equally, but owing to having sucked ethylene glycol in aqua oxidation film, this layer of boehmite is divided into the part showed increased that internal density is high and outer fiber shape part does not almost have, and this layer of hydrated film more easily changes into γ-AL2O3 when forming like this.Thereby the dielectric property of anode oxide film have been improved.
(2) utilize the etched foil that maleic acid is crossed hydration-treated to process, paillon foil seriously corroded when preventing from next adopting phosphoric acid and salt thereof to change into, finally solves the resistance to water problem of oxide-film.
(3) first secondarys change in processing and adopt phosphoric acid and salting liquid thereof to change into, be mainly to utilize phosphate radical to react with aluminium, further reaming is carried out in etched foil cavity, be beneficial to improve specific volume, because phosphoric acid film is thinner, can make the warpage intensity of Waste Acid From Hua Cheng Foil obviously improve simultaneously.
Etched foil through special processing is used the electrical performance data of the motor paper tinsel of this patent chemical synthesizing method and traditional chemical synthesizing method gained to be compared as follows:
| Chemical synthesizing method | Resistance to water Tr60 (S) | Warpage intensity (inferior) | Leakage current uA/5cm2 |
| This patent den process | 6-10 | 100-130 | 50-80 |
| Tradition den process | 10-45 | 60-80 | 98-120 |
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is elaborated.
Embodiment 1
A kind of anode foil manufacturing method for alternating current motor capacitor:
Hydration-treated: get pit for running through type, and the etched foil of average pore size 1.5 μ m, the ethylene glycol solution that is placed in concentration and is 0.1wt%, temperature and be 90 ℃ floods 5 minutes;
Change into preliminary treatment: in concentration, be 0.2wt% again, temperature is that the maleic acid solution processing time of 75 ℃ is 2 minutes;
Pyatyi changes into processing: taking out and to be placed in the phosphate that concentration is 0.1wt%, is 20mA/cm at 75 ℃, current density
2, under the voltage condition that is 100V, change into 10 minutes;
It is 0.05wt% that taking-up is placed in concentration, in the phosphate that temperature is 75 ℃, current density is 20mA/cm
2, under the voltage condition that is 200V, change into 10 minutes;
Take out washing 2 minutes; Be placed in again boric acid that concentration is 5wt% and 0.2wt% ammonium pentaborate, temperature and be the solution of 75 ℃, current density 20mA/cm
2, under the condition that voltage is 260V, change into 10 minutes;
After taking-up, be placed in again boric acid that concentration is 5wt% and 0.1wt% ammonium pentaborate, temperature and be the solution of 75 ℃, current density 20mA/cm
2, under the condition that voltage is 300V, change into 10 minutes;
After taking-up, be placed in again the solution of 75 ℃ of boric acid that concentration is 5wt% and 0.03wt% ammonium pentaborate, temperature, current density 20mA/cm
2, under the condition that voltage is 350V, change into 30 minutes;
Finally, take out etched foil and through conventional high-temperature heat treatment, depolarising processing, reparation, change into processing successively, in post-processing step, working concentration is that 0.1-5wt% phosphate solution floods, set temperature is 50-90 ℃, processing time is 1.5-4.5min, after reprocessing, adopt conventional drying and processing, generate the anode foils for alternating current motor capacitor.
The oxide-film dielectric property of the anode foils generating based on the present embodiment are good: leakage current is 76.7 uA/5cm
2; Resistance to hydrability is good: Tr60 is 6S; Warpage intensity 120 times.From SEM scanning electron microscopic observation, oxide-film surface does not almost have aqua oxidation film, can meet the needs that motor starting capacitor frequently discharges and recharges.
Embodiment 2
A kind of anode foil manufacturing method for alternating current motor capacitor:
Get pit for running through type, and the etched foil of average pore size 1.8 μ m, the ethylene glycol solution that is placed in concentration and is 0.5wt%, temperature and be 90 ℃ floods 5 minutes;
In concentration, be 0.2wt% again, temperature is that the maleic acid solution processing time of 75 ℃ is 2 minutes;
Taking-up is placed in phosphate that concentration is 0.1wt%, at 75 ℃, current density, is 20mA/cm
2, under the voltage condition that is 100V, change into 10 minutes;
It is 0.05wt% that taking-up is placed in concentration, in the phosphate that temperature is 75 ℃, current density is 20mA/cm
2, under the voltage condition that is 200V, change into 10 minutes;
Take out washing 2 minutes; Be placed in again boric acid that concentration is 5wt% and 0.2wt% ammonium pentaborate, temperature and be the solution of 75 ℃, current density 20mA/cm
2, under the condition that voltage is 260V, change into 10 minutes;
After taking-up, be placed in again boric acid that concentration is 5wt% and 0.1wt% ammonium pentaborate, temperature and be the solution of 75 ℃, current density 20mA/cm
2, under the condition that voltage is 300V, change into 10 minutes;
After taking-up, be placed in again the solution of 75 ℃ of boric acid that concentration is 5wt% and 0.03wt% ammonium pentaborate, temperature, current density 20mA/cm
2, under the condition that voltage is 350V, change into 30 minutes;
Finally, take out etched foil and through conventional high-temperature heat treatment, depolarising processing, reparation, change into processing successively, in post-processing step, working concentration is that 0.1-5wt% phosphate solution floods, set temperature is 50-90 ℃, processing time is 1.5-4.5min, after reprocessing, adopt conventional drying and processing, generate the anode foils for alternating current motor capacitor.
The oxide-film dielectric property of the anode foils generating based on the present embodiment are good: leakage current is 56.5 uA/5cm
2; Resistance to hydrability, Tr60 is 8S; Warpage intensity is 118 times.From SEM scanning electron microscopic observation, oxide-film surface does not almost have aqua oxidation film, can meet the needs that motor starting capacitor frequently discharges and recharges.
Embodiment 3
Under the working condition of embodiment 1, the concentration of the ethylene glycol solution in water and treatment step is controlled to 1.0wt%.
The oxide-film dielectric property of the anode foils generating based on the present embodiment are good, and leakage current is 57.3 uA/5cm
2; Resistance to hydrability is high, and Tr60 is 7S; Warpage intensity is 122 times.From SEM scanning electron microscopic observation, oxide-film surface does not almost have aqua oxidation film, can meet the needs that motor starting capacitor frequently discharges and recharges.
Embodiment 4
Under the working condition of embodiment 1, the concentration of the ethylene glycol solution in water and treatment step is controlled to 5.0wt%.
The oxide-film dielectric property of the anode foils generating based on the present embodiment are good, and leakage current is 56.3 uA/5cm
2; Resistance to hydrability is high, and Tr60 is 6S; Warpage intensity is 125 times, and from SEM scanning electron microscopic observation, oxide-film surface does not almost have aqua oxidation film, can meet the needs that motor starting capacitor frequently discharges and recharges.
Embodiment 5
Under the working condition of embodiment 1, the concentration of the ethylene glycol solution in water and treatment step is controlled to 10.0wt%.
The oxide-film dielectric property of the anode foils generating based on the present embodiment are good, and leakage current is 55.7 uA/5cm2; Resistance to hydrability is high, and Tr60 is 8S; Warpage intensity is 115 times.From SEM scanning electron microscopic observation, oxide-film surface does not almost have aqua oxidation film, can meet the needs that motor starting capacitor frequently discharges and recharges.
Embodiment 6
Under the working condition of embodiment 1, the concentration of the ethylene glycol solution in water and treatment step is controlled to 20.0wt%.
The oxide-film dielectric property of the anode foils generating based on the present embodiment are good, and leakage current is 55.8 uA/5cm2; Resistance to hydrability is high, and Tr60 is 10S; Warpage intensity is 112 times, and from SEM scanning electron microscopic observation, oxide-film surface does not almost have aqua oxidation film, can meet the needs that motor starting capacitor frequently discharges and recharges.
Embodiment 7
Under the working condition of embodiment 1, the concentration of the ethylene glycol solution in water and treatment step is controlled to 30.0wt%.
The oxide-film dielectric property of the anode foils generating based on the present embodiment are good, and leakage current is 57.5 uA/5cm2; Resistance to hydrability is high, and Tr60 is 8S; Warpage intensity is 123 times, and from SEM scanning electron microscopic observation, oxide-film surface does not almost have aqua oxidation film, can meet the needs that motor starting capacitor frequently discharges and recharges.
Embodiment 8
Under the working condition of embodiment 1, the concentration of the ethylene glycol solution in water and treatment step is controlled to 40.0wt%.
The oxide-film dielectric property leakage current of the anode foils generating based on the present embodiment is 55.6 uA/5cm2; The Tr60 of resistance to hydrability is 10S; Warpage intensity is 108 times.From SEM scanning electron microscopic observation, oxide-film surface does not almost have aqua oxidation film, can meet the needs that motor starting capacitor frequently discharges and recharges.
Comparative example 1
Get pit for running through type, and the etched foil of average pore size 1.5 μ m, the pure water solution that is placed in temperature and is 95 ℃ boils 5 minutes; In concentration, be 0.2wt% again, temperature is that the maleic acid solution processing time of 75 ℃ is 2 minutes;
Taking-up is placed in phosphate that concentration is 0.1wt%, at 75 ℃, current density, is 20mA/cm
2, under the voltage condition that is 100V, change into 10 minutes;
It is 0.05wt% that taking-up is placed in concentration, in the phosphate that temperature is 75 ℃, current density is 20mA/cm
2, under the voltage condition that is 200V, change into 10 minutes;
Take out washing 2 minutes; Be placed in again boric acid that concentration is 5wt% and 0.2wt% ammonium pentaborate, temperature and be the solution of 75 ℃, current density 20mA/cm
2, under the condition that voltage is 260V, change into 10 minutes;
After taking-up, be placed in again boric acid that concentration is 5wt% and 0.1wt% ammonium pentaborate, temperature and be the solution of 75 ℃, current density 20mA/cm
2, under the condition that voltage is 300V, change into 10 minutes;
After taking-up, be placed in again the solution of 75 ℃ of boric acid that concentration is 5wt% and 0.03wt% ammonium pentaborate, temperature, current density 20mA/cm
2, under the condition that voltage is 350V, change into 30 minutes;
Finally take out carry out high-temperature heat treatment, depolarising, change into again, reprocessing, oven dry, form anode foils.
The oxide-film dielectric property of anode foils that more than change into generation are poor, and leakage current is 120 uA/5cm greatly
2; Resistance to hydrability is poor, and Tr60 is 45S; Warpage intensity is only 75 times.
Comparative example 2
Get pit for running through type, and the etched foil of average pore size 1.8 μ m, the ethylene glycol solution that is placed in concentration and is 30wt%, temperature and be 90 ℃ floods 5 minutes;
Without maleic acid, process, be directly placed in phosphate that concentration is 0.1wt%, at 75 ℃, current density, be 20mA/cm
2, under the voltage condition that is 100V, change into 10 minutes;
It is 0.05wt% that taking-up is placed in concentration, in the phosphate that temperature is 75 ℃, current density is 20mA/cm
2, under the voltage condition that is 200V, change into 10 minutes;
Take out washing 2 minutes; Be placed in again boric acid that concentration is 5wt% and 0.2wt% ammonium pentaborate, temperature and be the solution of 75 ℃, current density 20mA/cm
2, under the condition that voltage is 260V, change into 10 minutes;
After taking-up, be placed in again boric acid that concentration is 5wt% and 0.1wt% ammonium pentaborate, temperature and be the solution of 75 ℃, current density 20mA/cm
2, under the condition that voltage is 300V, change into 10 minutes;
After taking-up, be placed in again the solution of 75 ℃ of boric acid that concentration is 5wt% and 0.03wt% ammonium pentaborate, temperature, current density 20mA/cm
2, under the condition that voltage is 350V, change into 30 minutes;
Finally take out carry out high-temperature heat treatment, depolarising, change into again, reprocessing, oven dry, form anode foils.
The oxide-film dielectric property of anode foils that more than change into generation are poor, and leakage current is 98 uA/5cm
2; The Tr60 of resistance to hydrability is 10S; Warpage intensity is only 65 times.
From embodiment 1 to embodiment 8, can find out:
(1) compare with comparative example, when leakage current reduces, capacity is substantially constant;
(2) when the concentration of ethylene glycol is 0.1wt%, leakage current and comparative example start to approach, and the concentration of ethylene glycol is 0.1wt% while being 40wt%, and capacity is compared with comparative example, declines a lot, and therefore, the optium concentration of ethylene glycol is 0.5wt%-30wt%.
(3) from comparative example 2, can find out: do not use maleic acid, with embodiment, compared capacity loss 12%, leakage current also rises to some extent simultaneously.Therefore, when the leading portion that makes spent glycol make anode foils is processed, also must use maleic acid solution to carry out pre-treatment for the second time, to prevent that aluminium foil from too corroding, cause the decline of capacity.
Claims (10)
1. the anode foil manufacturing method for alternating current motor capacitor, comprise that hydration-treated, Pyatyi change into processing, high-temperature heat treatment, depolarising and process, repair and change into processing, reprocessing and drying and processing, it is characterized in that: after described hydration-treated step, increase and change into pre-treatment step;
Described hydration-treated step is for adopting glycol water to carry out impregnation process; Be specially pit as running through type, and etched foils more than average pore size 1.5 μ m to put into concentration be 0.1-30wt%, temperature is impregnation process 1-10min in the ethylene glycol solution of 60-100 ℃;
Describedly change into pre-treatment step for etched foil that hydration-treated is crossed, to put into concentration be 0.01-0.5wt%, temperature is to carry out impregnation process in the maleic acid solution of 70-95 ℃, and the time that impregnation process is set is 10s-5min.
2. the anode foil manufacturing method for alternating current motor capacitor according to claim 1, is characterized in that: in described hydration-treated step ethylene glycol solution concentration be 0.5-30wt%.
3. the anode foil manufacturing method for alternating current motor capacitor according to claim 1, is characterized in that: it is aqueous phosphatic that described Pyatyi changes into the electrolyte that first and second grade in processing change into use.
4. the anode foil manufacturing method for alternating current motor capacitor according to claim 3, it is characterized in that: described one-level changes into process and is specially that to be placed in concentration be 0.01-0.3wt% by changing into pretreated etched foil, temperature is the aqueous phosphatic of 60-90 ℃, and it is 10-30mA/cm that current density is set
2, voltage is 30% seal making alive, changes into and processes 5-20min.
5. the anode foil manufacturing method for alternating current motor capacitor according to claim 3, it is characterized in that: described secondary changes into process to be specially and through one-level, changes into the etched foil of processing to be placed in concentration be 0.01-0.1wt%, in the phosphate solution of temperature 60-90 ℃, it is 10-30mA/cm that current density is set
2, the seal making alive that voltage is 60%, changes into and processes 5-20 minute.
6. the anode foil manufacturing method for alternating current motor capacitor according to claim 1, is characterized in that: it is that concentration is that boric acid and the concentration of 1-12wt% is the mixed solution of 0.01-0.2wt% ammonium pentaborate that described Pyatyi changes into electrolyte that third and fourth and Pyatyi in processing change into.
7. the anode foil manufacturing method for alternating current motor capacitor according to claim 5, is characterized in that: described the 3rd polarization is processed the etched foil being specially after two utmost point polarization are processed and taken out washing 2 minutes; Be placed in again boric acid and 0.01-0.2wt% ammonium pentaborate mixed solution that concentration is 1-12wt%, set temperature 60-90 ℃, current density 10-30mA/cm
2, the seal making alive that voltage is 78%, changes into and processes 5-20 minute.
8. the anode foil manufacturing method for alternating current motor capacitor according to claim 5, it is characterized in that: described the 4th polarization is processed after the etched foil being specially after three utmost point polarization are processed takes out and is placed in boric acid and the 0.01-0.1wt% ammonium pentaborate mixed solution that concentration is 1-10wt% again, set temperature 60-90 ℃, current density 10-30mA/cm
2, the seal making alive that voltage is 90%, changes into and processes 5-20 minute.
9. the anode foil manufacturing method for alternating current motor capacitor according to claim 5, it is characterized in that: described the 5th polarization is processed after the etched foil being specially after four utmost point polarization are processed takes out and is placed in boric acid and the 0.01-0.06wt% ammonium pentaborate mixed solution that concentration is 1-10wt% again, solution temperature 60-90 ℃ is set, current density 10-30mA/cm
2, the seal making alive that voltage is 100%, changes into and processes 15-60 minute.
10. the anode foil manufacturing method for alternating current motor capacitor according to claim 1, is characterized in that: described reprocessing is for being used phosphate solution to flood, and set temperature is 50-90 ℃, and the processing time is 1.5-4.5min; The concentration of described phosphate solution is 0.1-5wt%.
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| 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 |
| CN110144612A (en) * | 2019-04-12 | 2019-08-20 | 浙江丰川电子科技有限公司 | A kind of anode foils chemical synthesis technology |
| CN112071648A (en) * | 2020-07-13 | 2020-12-11 | 新疆众和股份有限公司 | Five-stage phosphate formation process |
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