CN103779098B - Formation method of energy storage material applied to alternating current motor start capacitor - Google Patents
Formation method of energy storage material applied to alternating current motor start capacitor Download PDFInfo
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- CN103779098B CN103779098B CN201410004956.9A CN201410004956A CN103779098B CN 103779098 B CN103779098 B CN 103779098B CN 201410004956 A CN201410004956 A CN 201410004956A CN 103779098 B CN103779098 B CN 103779098B
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Abstract
The invention provides a formation method of an energy storage material applied to an alternating current motor start capacitor. The formation method comprises the steps that pre-forming is carried out on a through type corrosion foil in an oxalic acid solution, wherein the voltage is 2 to 10V, and the forming time is 1 to 5min; pre-forming is carried out; rinsing and boiling are carried out; three level formation is carried out in formation liquid composed of azelaic acid of 0.1 to 1.0g/L and ammonium hydrogen azelate of 0.5 to 1.5g/L to reach required voltage; heat processing is carried out, wherein the temperature is 200 to 400 DEG C and the processing time is 1 to 3min; and phosphate processing, formation repairing and drying are carried out. The energy storage material produced by using the method has the characteristics of low loss, good hydration resistance, and good ripple current impact resistance and temperature rise resistance, and is suitable for the energy storage material of the alternating current motor start capacitor.
Description
Technical field
The present invention relates to a kind of chemical synthesizing method of alternating current motor start-up capacitance energy storage material.
Background technology
The preparation method of conventional aluminium electrolutic capacitor energy storage material, generally comprise boiling water treating, multistage chemical conversion, heat at
Manage, be melted into again, phosphoric acid processes, is melted into, post processing.Chemical conversion temperature height (more than 85 DEG C), heat treatment temperature are high（More than 450
℃）, obtain the good mold oxide film of densification, insulating properties.This energy storage material has laminboard layer non-penetrating type pore space structure, electricity
Capacity is big, loss tangent（tgδ）High, oxide-film resistance to ripple current impact and resistance to temperature characteristic relatively poor it is impossible to full
The needs of sufficient alternating current motor start-up capacitance device.
The alternating current that alternating current motor start-up capacitance device is circulated is very big, has=U according to P2 ~ω Ctg δ, if tg δ is big,
Short time internal heat generation power is just big, and capacitor is brought rapidly up leading to inside to be exitted in a large number and rouses bottom and even pop.Therefore medium
Loss is little, and the exchange impact tolerance in the short time requires higher i.e. life characteristics to want quite stable.
Content of the invention
It is an object of the invention to provide a kind of chemical synthesizing method of alternating current motor start-up capacitance energy storage material, using this method
The energy storage material producing has the characteristics that loss is low, good, the resistance to ripple current of resistance to hydrability impacts and resistance to temperature characteristic is good, is suitable for using
In alternating current motor start-up capacitance energy storage material.
The technical solution of the present invention is:A kind of chemical synthesizing method of alternating current motor start-up capacitance energy storage material, will pass through
Flow-through etched foil oxalic acid solution concentration be 25g/L, voltage 2～10V, electric current density be 20mA/cm2, temperature be 20 DEG C of conditions
Under carry out pre-formed 1～5min, then clean up, 95 DEG C of pure water boil 1～4min, then in Azelaic Acid 0.1～1.0g/
Carry out three-level chemical conversion respectively, chemical conversion temperature is 70～80 DEG C, changes in the forming liquid of L and Azelaic Acid hydrogen ammonium 0.5～1.5g/L composition
One-tenth electric current density is 10～20mA/cm2, constant 6～24min when reaching setting voltage, then heat treatment 1 at 300～400 DEG C
～3min, then be melted into reparation 5～8min, then volume ratio be 3% phosphoric acid solution in process 2～6min in 75 DEG C, then be melted into
Repair 5～8min, then volume ratio be 3% phosphoric acid solution in 70 DEG C process 1～3min, heat treatment 1 at 200～300 DEG C
～3min, then it is melted into reparation 5～8min, dry.
The voltage request of described three-level chemical conversion is assigned as 30～40%, 60～70%, 100%.
The present invention compared with prior art has the advantage that and effect:
1. adopt the pre-formed operation of oxalic acid, then boiling pure water is melted into again, can obtain long-life energy storage material.
2. process is boiled using the short time, generate relatively thin aqua oxidation film, be different from conventional energy storage material and boil for a long time
Boiling is processed, and generates thicker aqua oxidation film.
3. use through etched foil, low temperature chemical conversion, heat treatment temperature are relatively low and prepared amorphous（Armorphous）Oxide-film
Energy storage material, has the characteristics that loss is low, resistance to ripple current impacts and resistance to temperature characteristic is good.Being different from conventional energy storage material has folder
Sandwich layer, crystal formation oxide-film.
4. adopt 2 hypophosphorous acid to process, the resistance to hydrability of oxide-film is good, energy storage material stable performance.
Specific embodiment:
With reference to embodiment, technical scheme is described in further detail, but embodiments of the present invention do not limit
In this.
Embodiment 1
One example of the chemical synthesizing method of alternating current motor start-up capacitance energy storage material of the present invention, walks including following
Suddenly：Take through etched foil oxalic acid solution concentration be 25g/L, voltage be 2V, electric current density be 20mA/cm2, temperature be 20 DEG C
Under the conditions of carry out pre-formed 1min, taking-up cleans up, and boils 1min in 95 DEG C of pure water, then in Azelaic Acid 1.0g/L and nonyl two
In the forming liquid of sour hydrogen ammonium 1.5g/L composition, it is 70 DEG C, electric current density 10mA/cm in temperature2, voltage be 70V under the conditions of carry out
The first order is melted into, and constant voltage time is 8min；With phase in the forming liquid of Azelaic Acid 0.8g/L and Azelaic Acid hydrogen ammonium 1.2g/L composition
Same condition carries out second level chemical conversion, and voltage rises to 140V, constant voltage 8min；Then in Azelaic Acid 0.6g/L and Azelaic Acid hydrogen ammonium
In the forming liquid of 1.0g/L composition, third level chemical conversion is carried out with identical condition, voltage rises to 200V, constant voltage 16min；Then exist
Heat treatment 1min at 300 DEG C, then the chemical conversion of 200V constant voltage repairs 6min, then processes 1min at 75 DEG C of 3% phosphoric acid solution, then
6min is repaired in the chemical conversion of 200V constant voltage, then processes 1min at 70 DEG C of 3% phosphoric acid solution, then carries out heat treatment at 200 DEG C
1min, then 200V constant voltage chemical conversion reparation 6min, finally take out and dry 2min.
The relevant parameter of energy storage material during table 1200Vf chemical conversion
| tgδ | Tr600, (s) | |
| Commonly | 0.045 | 38 |
| The present invention | 0.036 | 13 |
Find out from embodiment 1 result, using the present invention than prior art energy storage material loss tangent（tgδ）Little
20%th, pressure rising time Tr after resistance to hydration（600）Shorten 66%.
Embodiment 2
Another example of the chemical synthesizing method of alternating current motor start-up capacitance energy storage material of the present invention, walks including following
Suddenly：Take through etched foil oxalic acid solution concentration be 25g/L, voltage 5V, electric current density be 20mA/cm2, temperature be 20 DEG C of bars
Carry out pre-formed 2min, taking-up cleans up, and boils 2min in 95 DEG C of pure water, in Azelaic Acid 0.8g/L and Azelaic Acid hydrogen ammonium under part
The forming liquid of 1.2g/L composition, is 75 DEG C, electric current density 15mA/cm in temperature2, voltage be 120V under the conditions of carry out the first order
Become, constant voltage time is 10min；With identical condition in the forming liquid of Azelaic Acid 0.6g/L and Azelaic Acid hydrogen ammonium 1.0g/L composition
Carry out second level chemical conversion, voltage rises to 240V, constant voltage 10min；Then in Azelaic Acid 0.4g/L and Azelaic Acid hydrogen ammonium 0.8g/L group
In the forming liquid becoming, third level chemical conversion is carried out with identical condition, voltage rises to 340V, constant voltage 20min；Then by paillon foil 350
Carry out heat treatment 2min at DEG C, then 8min is repaired in the chemical conversion of 340V constant voltage, then processes 3min at 75 DEG C of 3% phosphoric acid solution, then
8min is repaired in the chemical conversion of 340V constant voltage, and paillon foil then carries out at 250 DEG C heat treatment 1.5min, then in 70 DEG C of 3% phosphoric acid solution
Lower process 2min, then 340V constant voltage chemical conversion reparation 8min, finally take out and dry 2min.
The relevant parameter of energy storage material during table 2340Vf chemical conversion
| tgδ | Tr600, (s) | |
| Commonly | 0.036 | 45 |
| The present invention | 0.025 | 16 |
Find out from embodiment 2 result, using the present invention than prior art energy storage material loss tangent（tgδ）Little
28%th, pressure rising time Tr after resistance to hydration（600）Shorten 64%.
Embodiment 3
Another example of the chemical synthesizing method of alternating current motor start-up capacitance energy storage material of the present invention, including as follows
Step：Take through etched foil oxalic acid solution concentration be 25g/L, voltage 10V, electric current density be 20mA/cm2, temperature be 20
Carry out pre-formed 5min, taking-up cleans up, and boils 4min in 95 DEG C of pure water, in Azelaic Acid 0.4g/L and Azelaic Acid under the conditions of DEG C
In the forming liquid of hydrogen ammonium 1.0g/L composition, it is 80 DEG C, electric current density 20mA/cm in temperature2, voltage be to carry out the under the conditions of 200V
One-level is melted into, and constant voltage time is 12min；In the forming liquid of Azelaic Acid 0.2g/L and Azelaic Acid hydrogen ammonium 0.8g/L composition, with identical
Condition carry out second level chemical conversion, voltage rises to 400V, constant voltage 12min；Then in Azelaic Acid 0.1g/L and Azelaic Acid hydrogen ammonium
The forming liquid of 0.5g/L composition, carries out third level chemical conversion with identical condition, voltage rises to 560V, constant voltage 24min；Then by paper tinsel
Piece carries out heat treatment 3min at 400 DEG C, then 10min is repaired in the chemical conversion of 560V constant voltage, then processes at 75 DEG C of 3% phosphoric acid solution
6min, then the chemical conversion of 560V constant voltage repairs 10min, then processes 3min at 70 DEG C of 3% phosphoric acid solution, then by paillon foil at 300 DEG C
Under carry out heat treatment 3min, then 560V constant voltage chemical conversion repair 10min, finally take out dry 2min.
The relevant parameter of energy storage material during table 3560Vf chemical conversion
| tgδ | Tr600, (s) | |
| Commonly | 0.026 | 56 |
| The present invention | 0.022 | 28 |
Find out from embodiment 3 result, using the present invention than prior art energy storage material loss tangent（tgδ）Little
15%th, pressure rising time Tr after resistance to hydration（600）Shorten 50%.
Claims (1)
1. a kind of chemical synthesizing method of alternating current motor start-up capacitance energy storage material is it is characterised in that comprise the steps：By insertion
Type etched foil oxalic acid solution concentration be 25g/L, voltage 2～10V, electric current density be 20mA/cm2, temperature be 20 DEG C under the conditions of
Carry out pre-formed 1～5min, then clean up, 95 DEG C of pure water boil 1～4min, then in Azelaic Acid 0.1～1.0 g/L
And in the forming liquid of Azelaic Acid hydrogen ammonium 0.5～1.5 g/L composition, carrying out three-level chemical conversion respectively, chemical conversion temperature is 70～80 DEG C, changes
One-tenth electric current density is 10～20mA/cm2, constant 6～24min when reaching setting voltage, then heat treatment 1 at 300～400 DEG C
～3min, then be melted into reparation 5～8min, then volume ratio be 3% phosphoric acid solution in process 2～6min in 75 DEG C, then change
Become reparation 5～8min, then volume ratio be 3% phosphoric acid solution in 70 DEG C process 1～3min, at heat at 200～300 DEG C
Reason 1～3min, then it is melted into reparation 5～8min, dry.
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| CN114496570A (en) * | 2021-12-29 | 2022-05-13 | 广西贺州市桂东电子科技有限责任公司 | Preparation method of anode foil for rapidly charging and discharging aluminum electrolytic capacitor |
| CN114334460A (en) * | 2021-12-30 | 2022-04-12 | 贵州师范学院 | Method for improving large ripple current tolerance of tantalum electrolytic capacitor |
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| US4547275A (en) * | 1984-02-03 | 1985-10-15 | Showa Aluminum Kabushiki Kaisha | Process for treating surface of aluminum foil for use as electrode of electrolytic capacitors |
| CN2466772Y (en) * | 2001-02-27 | 2001-12-19 | 上海汇龙仪表电子有限责任公司天和电极箔分公司 | Multi-stage AC silver foil band corrosion device |
| CN1990914A (en) * | 2005-12-30 | 2007-07-04 | 新疆众和股份有限公司 | Forming technique for reducing voltage rising time of aluminum electrolytic capacitor anode foil |
| CN101030487A (en) * | 2006-12-22 | 2007-09-05 | 东莞市东阳光电容器有限公司 | Production of electrolytic capacitor anode aluminum foil |
| EP1873268A1 (en) * | 2005-03-17 | 2008-01-02 | Denko Kabushiki Kaisha Showa | Process for producing aluminum material for electrolytic capacitor electrode, aluminum material for electrolytic capacitor electrode, process for producing electrolytic capacitor electrode material, anode material for aluminum electrolytic capacitor, and aluminum electrolytic capacitor |
| CN101707141A (en) * | 2009-11-09 | 2010-05-12 | 广西贺州市桂东电子科技有限责任公司 | Method for manufacturing anodic foil of aluminum electrolytic capacitor |
| CN103227052A (en) * | 2013-01-09 | 2013-07-31 | 朱健雄 | Method for manufacturing medium-high voltage aluminum electrolytic capacitor |
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2014
- 2014-01-06 CN CN201410004956.9A patent/CN103779098B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4547275A (en) * | 1984-02-03 | 1985-10-15 | Showa Aluminum Kabushiki Kaisha | Process for treating surface of aluminum foil for use as electrode of electrolytic capacitors |
| CN2466772Y (en) * | 2001-02-27 | 2001-12-19 | 上海汇龙仪表电子有限责任公司天和电极箔分公司 | Multi-stage AC silver foil band corrosion device |
| EP1873268A1 (en) * | 2005-03-17 | 2008-01-02 | Denko Kabushiki Kaisha Showa | Process for producing aluminum material for electrolytic capacitor electrode, aluminum material for electrolytic capacitor electrode, process for producing electrolytic capacitor electrode material, anode material for aluminum electrolytic capacitor, and aluminum electrolytic capacitor |
| CN1990914A (en) * | 2005-12-30 | 2007-07-04 | 新疆众和股份有限公司 | Forming technique for reducing voltage rising time of aluminum electrolytic capacitor anode foil |
| CN101030487A (en) * | 2006-12-22 | 2007-09-05 | 东莞市东阳光电容器有限公司 | Production of electrolytic capacitor anode aluminum foil |
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