CN101425387B - Extending corrosion method for low voltage anode aluminum foil - Google Patents
Extending corrosion method for low voltage anode aluminum foil Download PDFInfo
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- CN101425387B CN101425387B CN2008100297968A CN200810029796A CN101425387B CN 101425387 B CN101425387 B CN 101425387B CN 2008100297968 A CN2008100297968 A CN 2008100297968A CN 200810029796 A CN200810029796 A CN 200810029796A CN 101425387 B CN101425387 B CN 101425387B
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Abstract
The invention relates to the technical field of a preparation method of aluminum foil, in particular to an extended-surface corrosion method of low-voltage anode aluminum foil. The extended-surface corrosion method comprises choice of original low-voltage light foil and electrochemical corrosion, wherein unannealed hard-state aluminum foil is selected for the original low-voltage light foil, and the degree of cubic texture of the unannealed hard-state aluminum foil can not be more than 50 percent; the electrochemical corrosion comprises twice etchings, and the used current is both 50 Hz power frequency AC current. The invention has simple technology and equipment, and the anode foil products have high capacitance and good strength.
Description
Technical field:
The present invention relates to the aluminum foil preparation technical field, particularly extending corrosion method for low voltage anode aluminum foil.
Background technology
The anode of aluminium electrolytic capacitor is a high-purity aluminum foil, the capacitance of capacitor is directly proportional with the real surface of capacitor electrode material is long-pending, the real surface of capacitor electrode material is long-pending big more, then the capacitance of capacitor is also big more, under the certain situation of condenser capacity, the employed electrode material of capacitor is few more, and the volume of capacitor is correspondingly also just more little, thereby provides condition for the miniaturization of electronic instrument.Long-pending for the real surface that increases the electrode aluminium foil, generally the method by corrosion forms a large amount of tiny pits at aluminium foil surface, and the real surface that enlarges aluminium foil is long-pending.
The expansion face corrosion of low voltage anode aluminum foil, domesticly generally adopt 50 hertz industrial-frequency alternating current stream to corrode, generally in the solution that comprises hydrochloric acid and other additives, carry out, because it is inappropriate that additive is selected, the capacitance of aluminium foil is generally not high, the external general frequency-changing AC electricity that adopts is produced low voltage anode aluminum foil, and this method gained anode foils capacitance is higher, but production cost is also very high.
Summary of the invention:
Purpose of the present invention is at the deficiencies in the prior art, and it is simple, with low cost to disclose a kind of technology, low voltage anode aluminum foil capacitance height that makes and the good extending corrosion method for low voltage anode aluminum foil of mechanical strength.
The objective of the invention is to be achieved by the following method:
A kind of extending corrosion method for low voltage anode aluminum foil comprises the selection and the electrochemical corrosion of the former smooth paper tinsel of low pressure; The former smooth paper tinsel of described low pressure is selected unannealed hard attitude aluminium foil, and hard attitude aluminium foil cubic texture degree can not be greater than 50%; Electrochemical corrosion is twice corrosion, and use therein electric current is 50 hertz industrial frequency AC electric current.
Wherein, in described twice electrochemical corrosion, for the first time electrochemical corrosion is to carry out in the mixed solution that comprises hydrochloric acid and sulfuric acid, the concentration of hydrochloric acid is controlled at 15～25%, sulfuric acid concentration is controlled at 0.1～1%, and corrosion temperature is 33～43 degree, and current density is 0.1～0.4A/cm
2
In described twice electrochemical corrosion, for the second time electrochemical corrosion is to comprise hydrochloric acid, carry out in the mixed solution of sulfuric acid and oxalic acid, the concentration of hydrochloric acid is controlled at 15～25%, sulfuric acid concentration is controlled at 0.1～2%, concentration of oxalic acid is controlled at 8～20g/L, and corrosion temperature is 33～43 degree, and current density is 0.1～0.7A/cm
2
Below the principle of the invention is done detailed description: the two-stage electrochemical corrosion of low voltage anode aluminum foil, wherein the purpose of for the first time electrochemical corrosion is to form a large amount of evenly tiny pits at aluminium foil surface, for the second time electrochemical corrosion be in front the pit basis further to the corrosion of aluminium foil depth direction, form fine and closely woven cellular hole.The electrochemical corrosion first time of the present invention is to carry out in the mixed solution that comprises hydrochloric acid and sulfuric acid, because corrosion temperature is very low, be controlled at the 33-43 degree, pit preferentially takes place at the crystal grain intersection of aluminium foil surface, belong to the grain boundary corrosion type, therefore the cubic texture degree of former smooth paper tinsel is high more, crystal is described, and { 100} structural plane proportion is big more, then the number of tunnel type straight hole is many more, change into paper tinsel if be used for high pressure, then favourable to improving specific volume, but concerning low-pressure chemical synthesis foil, it is more a lot of greatly than the surface area of tunnel type hole to form cellular hole, therefore the low more light paper tinsel of cubic texture degree can be high more with the prepared low-voltage anode foil capacitance of technology of the present invention, Given this reason, the cubic texture degree of the former smooth paper tinsel of the present invention must could obtain abundant initial pit less than 50% in the electrochemical corrosion first time.
For the first time electrochemical corrosion is to carry out in the mixed solution that comprises hydrochloric acid and sulfuric acid, and the concentration of hydrochloric acid is controlled at 15～25%, and sulfuric acid concentration is controlled at 0.1～1%, and corrosion temperature is 33～43 degree, and current density is controlled at 0.1～0.4A/cm
2The effect of hydrochloric acid provides chloride ion aluminium foil surface is corroded, and the effect of sulfuric acid is to be adsorbed on aluminium foil and certain protection is played on the hole surface.Corrosive effect and hydrochloric acid and sulfuric acid concentration, corrosion temperature and current density are relevant.Concentration of hydrochloric acid is lower than at 15% o'clock, aluminium foil surface pit quantity seldom, capacitance is low, concentration of hydrochloric acid is higher than at 25% o'clock, aluminium foil surface is from seriously corroded, intensity reduces, capacitance is also low; Sulfuric acid concentration is lower than at 0.1% o'clock, and the aluminium foil surface protection is not enough, has a lot of apertures to merge, and capacitance is low, and sulfuric acid concentration is higher than at 1% o'clock, and the aluminium foil surface protection excessively reduces chloride ion activity, the pit decreased number, and capacitance is low; When solution temperature less than 33 was spent, corrosion reaction speed was slow, and corrosion efficient is low, and capacitance is low, and solution temperature is higher than 43 when spending, and aluminium foil is from seriously corroded, and capacitance is also low; Current density is lower than 0.1A/cm
2, aluminium foil face-expanding is inhomogeneous, and the pit number is few, and capacitance is low, and current density is higher than 0.4A/cm
2, the aluminium foil surface pit is too much, and hole merges serious, and capacitance is low.
For the second time electrochemical corrosion is to comprise hydrochloric acid, carries out in the mixed solution of sulfuric acid and oxalic acid, and the concentration of hydrochloric acid is controlled at 15～25t%, sulfuric acid concentration is controlled at 0.1～2%, concentration of oxalic acid is controlled at 8～20 grams per liters, and corrosion temperature is 33～43 degree, current density 0.1～0.7A/cm
2Wherein sulfuric acid and oxalic acid play a part crucially, and the hole that they have formed as additive protection aluminium foil surface together also reduces the phenomenon that hole merges.Concentration of hydrochloric acid is lower than at 15% o'clock, and chlorine ion concentration is low, and activity is very low, and the pit of aluminium foil surface is just few, and capacitance is low, and concentration of hydrochloric acid is higher than at 25% o'clock, and aluminium foil surface is from seriously corroded, the aluminium foil attenuate, and the blackout dry linting, capacitance is also low; Sulfuric acid concentration is lower than at 0.1% o'clock, and the aluminium foil surface protection is not enough, and capacitance is low, and sulfuric acid concentration is higher than at 2% o'clock, and the aluminium foil surface protection is excessive, the pit decreased number, and capacitance is low; When concentration of oxalic acid was lower than 8g/L, the protection of aluminium foil hole was not enough, and the phenomenon that a large amount of holes merge can take place, and capacitance is low, and when concentration of oxalic acid was higher than 20g/L, too much oxalate covered aluminium foil surface, had hindered the generation of new pit, and capacitance is also low; When solution temperature less than 33 was spent, corrosion reaction speed was slow, and corrosion efficient is low, and capacitance is low, and solution temperature is higher than 43 when spending, and aluminium foil is from seriously corroded, and capacitance is also low; Current density is lower than 0.1A/cm
2, the pit number is few, and capacitance is low, and current density is higher than 0.7A/cm
2, the aluminium foil surface pit is too much, and hole merges in a large number, the blackout dry linting, capacitance is low.
Beneficial effect of the present invention is: by choose reasonable and twice electrochemical corrosion to former smooth paper tinsel, to obtain to have the low voltage anode aluminum foil of bigger true surface area and better mechanical strength.
Embodiment:
The following examples can be used for making those skilled in the art more fully to understand the present invention, but do not limit the present invention in any way.
Embodiment 1:
Be that 50% the unannealed smooth paper tinsel of low pressure carries out twice electrochemical corrosion to cube texture, 50 hertz industrial-frequency alternating current is all adopted in twice corrosion, for the first time electrochemical corrosion is to carry out in the sulfuric acid mixed solution of 15% hydrochloric acid and 0.1%, corrosion temperature is 33 degree, and current density is controlled at 0.1A/cm
2, for the second time electrochemical corrosion is the hydrochloric acid at 15wt%, carries out in the oxalic acid mixed solution of 0.1% sulfuric acid and 8g/L, and corrosion temperature is 33 degree, and current density is controlled at 0.3A/cm
2
Embodiment 2:
Be that 41% the unannealed smooth paper tinsel of low pressure carries out twice electrochemical corrosion to cube texture, 50 hertz industrial-frequency alternating current is all adopted in twice corrosion, for the first time electrochemical corrosion is to carry out in the sulfuric acid mixed solution of 25% hydrochloric acid and 1%, and corrosion temperature is 43 degree, and current density is controlled at 0.4A/cm
2, for the second time electrochemical corrosion is the hydrochloric acid 25%, carries out in the oxalic acid mixed solution of 2% sulfuric acid and 20g/L, and corrosion temperature is 33 degree, and current density is controlled at 0.7A/cm
2
Embodiment 3:
Be that 28% the unannealed smooth paper tinsel of low pressure carries out twice electrochemical corrosion to cube texture, 50 hertz industrial-frequency alternating current is all adopted in twice corrosion, for the first time electrochemical corrosion is to carry out in the sulfuric acid mixed solution of 20% hydrochloric acid and 0.5%, corrosion temperature is 36 degree, and current density is controlled at 0.2A/cm
2, for the second time electrochemical corrosion is the hydrochloric acid 20%, carries out in the oxalic acid mixed solution of 1% sulfuric acid and 12g/L, and corrosion temperature is 33 degree, and current density is controlled at 0.4A/cm
2
Embodiment 4:
Be that 28% the unannealed smooth paper tinsel of low pressure carries out twice electrochemical corrosion to cube texture, 50 hertz industrial-frequency alternating current is all adopted in twice corrosion, for the first time electrochemical corrosion is to carry out in the sulfuric acid mixed solution of 15% hydrochloric acid and 0.5%, corrosion temperature is 33 degree, and current density is controlled at 0.2A/cm
2, for the second time electrochemical corrosion is the hydrochloric acid 20%, carries out in the oxalic acid mixed solution of 1% sulfuric acid and 18 grams per liters, and corrosion temperature is 33 degree, and current density is controlled at 0.3A/cm
2
The aluminium foil that the foregoing description is made cleans up, and changes under 20V and surveys its capacitance and tensile strength then, calculates aluminium foil capacitance tolerance rate and pulling force deviation ratio with respect to the prior art preparation, and the result is as shown in table 1 below:
Table 1:
| Rate of change of capacitance, % (20V changes into) | The pulling force deviation ratio, % | |
| Prior art | 100 | 100 |
| Embodiment 1 | 109 | 112 |
| Embodiment 2 | 111 | 109 |
| Embodiment 3 | 115 | 106 |
| Embodiment 4 | 114 | 107 |
Contrast by table 1 can find out that compared with the prior art the present invention has following advantage:
1, corrosion current of the present invention adopts 50 hertz industrial-frequency alternating current, can directly insert from electrical network, saved process and the equipment of electric current frequency conversion or shaping, so technology and equipment is simple, and production cost is low.
2, shown in subordinate list, capacitance of the present invention improves more than 9% than prior art, and high person reaches 15%.
3, shown in subordinate list, pulling force of the present invention improves more than 6% than prior art, and high person reaches 12%.
Claims (2)
1. extending corrosion method for low voltage anode aluminum foil comprises selection and the electrochemical corrosion of the former smooth paper tinsel of low pressure; It is characterized in that the former smooth paper tinsel of described low pressure is selected unannealed hard attitude aluminium foil, and hard attitude aluminium foil cube texture can not be greater than 50%; Electrochemical corrosion is twice corrosion, and the electric current that uses is 50 hertz industrial frequency AC electric current, for the first time electrochemical corrosion is to carry out in the mixed solution that comprises hydrochloric acid and sulfuric acid, the concentration of hydrochloric acid is controlled at 15～25%, sulfuric acid concentration is controlled at 0.1～1%, corrosion temperature is 33～43 degree, and current density is 0.1～0.4A/cm
2
2. extending corrosion method for low voltage anode aluminum foil according to claim 1, it is characterized in that, in described twice electrochemical corrosion, for the second time electrochemical corrosion is to carry out in the mixed solution that comprises hydrochloric acid, sulfuric acid and oxalic acid, the concentration of hydrochloric acid is controlled at 15～25%, and sulfuric acid concentration is controlled at 0.1～2%, and concentration of oxalic acid is controlled at 8～20g/L, corrosion temperature is 33～43 degree, and current density is 0.1～0.7A/cm
2
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| CN2008100297968A CN101425387B (en) | 2008-07-29 | 2008-07-29 | Extending corrosion method for low voltage anode aluminum foil |
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| CN2008100297968A CN101425387B (en) | 2008-07-29 | 2008-07-29 | Extending corrosion method for low voltage anode aluminum foil |
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| CN101425387B true CN101425387B (en) | 2010-12-08 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103187176B (en) * | 2013-03-22 | 2015-12-02 | 常州大学 | A kind of etching process of anode aluminum foil of electrolytic capacitor |
| CN110517892B (en) * | 2019-09-18 | 2021-01-26 | 南通海星电子股份有限公司 | Method for manufacturing electrode foil for solid aluminum electrolytic capacitor |
| CN118448167B (en) * | 2024-01-18 | 2024-10-18 | 南通南辉电子材料股份有限公司 | Medium-pressure corrosion foil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1920114A (en) * | 2006-08-02 | 2007-02-28 | 扬州宏远电子有限公司 | Corrosion method of anode foil for low-voltage aluminum electrolytic capacitor |
| CN1975949A (en) * | 2006-11-27 | 2007-06-06 | 乳源东阳光精箔有限公司 | Aluminium foil for electrolytic capacitor low-voltage anode use and producing method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1920114A (en) * | 2006-08-02 | 2007-02-28 | 扬州宏远电子有限公司 | Corrosion method of anode foil for low-voltage aluminum electrolytic capacitor |
| CN1975949A (en) * | 2006-11-27 | 2007-06-06 | 乳源东阳光精箔有限公司 | Aluminium foil for electrolytic capacitor low-voltage anode use and producing method thereof |
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