CN115725915B - Optical foil grain control method and preparation method of anode foil for electrolytic capacitor - Google Patents
Optical foil grain control method and preparation method of anode foil for electrolytic capacitor Download PDFInfo
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Abstract
The invention discloses a control method of optical foil crystal grains and a preparation method of anode foil for an electrolytic capacitor, and relates to the technical field of electrolytic capacitors. The control method of the optical foil crystal grain comprises the following steps: s1, placing a photo-foil sample into an annealing furnace, vacuumizing the annealing furnace to a vacuum degree of 50-100 Pa, quickly heating to 250 ℃, vacuumizing to a vacuum degree of less than or equal to 2Pa, preserving heat for 2h, S2, maintaining the vacuum degree, quickly heating to 420 ℃, continuously filling inert gas into the furnace at the vacuum degree, and preserving heat for 2-4h at a flow rate of 3-10L/min; s3, slowly cooling to 250 ℃, charging air to maintain normal atmospheric pressure, then rapidly cooling to 50-120 ℃ and discharging. The control method of the optical foil crystal grain realizes the control of the size and uniformity of the crystal grain through the control of the vacuum degree and the heating rate in the annealing process, and further improves the specific volume and the strength of the corrosion foil.
Description
Technical Field
The invention relates to the technical field of electrolytic capacitors, in particular to a photo-foil grain control method and a preparation method of anode foil for an electrolytic capacitor.
Background
An aluminum electrolytic capacitor is an energy storage element widely applied to the electronic and electric industry, and an anode foil for the aluminum electrolytic capacitor is an important raw material, and the structural characteristics of the anode foil determine the electrical performance of the aluminum electrolytic capacitor. Under the same corrosion process, products produced by different aluminum optical foils are different, the process level and the technical characteristics of aluminum optical foil production are reflected, aiming at different product requirements, the optical foil process for improving the corrosion specific volume by adding trace elements is provided, the corrosion speed is controlled by controlling the purity of optical foil aluminum, and the starting hole density is controlled by a crystal structure, but the requirements of the processes on the original aluminum ingot are too high, the realized threshold is also high, the requirements on the technical and production control level of a production enterprise are more, and the quality stability of the product is not well controlled. For example, the process of adding and controlling trace elements is controlled to be tens ppm level, and the main element iron, silicon and copper has higher purification technical requirements on aluminum ingots; besides high requirements on raw materials, the aluminum purity of the optical foil is controlled, the production and processing processes are strictly controlled, other impurities are prevented from being immersed and remained, and the inert gas dehydrogenation process is reinforced to eliminate hydrogen elements remained in aluminum, so that hydrogen embrittlement or bubbles in the aluminum layer after hydrogen aggregation in the later corrosion process are prevented, and the strength of the aluminum core is influenced. Moreover, these methods have mainly improved specific volume after corrosion, and do not have both specific volume and strength.
The conventional optical foil annealing scheme is divided into two schemes of inert gas protection annealing and vacuum annealing. The inert gas protection annealing is characterized by high speed, low cost and uniform temperature of the inner layer and the outer layer of the aluminum foil coil, and has the defects that the pressure between the layers of the aluminum foil coil is large, so that water oil vapor cannot be discharged, the hydrogen removal effect is poor, and even if part of water vapor is changed into hydrogen, hydrogen permeates into the aluminum foil, so that the strength of the aluminum foil is poor; the vacuum annealing has the advantages of good dehydrogenation effect, overlong annealing time, two times longer than that of inert gas protection annealing, slower heat conduction of the inner layer and the outer layer of the vacuum annealing, and adhesion of foil caused under the condition of unsmooth water and oil vapor discharge of the inner layer. The prior art discloses a finished product annealing method for improving the cubic texture of a high-voltage anode electronic aluminum foil, which is characterized in that a vacuum annealing mode under the protection of inert gas is adopted, so that the heating rate of an aluminum foil coil in the annealing process is accelerated, the growth blocking temperature section of the cubic texture is quickly passed, the influence is reduced, the occupancy of the cubic texture is improved, but the annealing mode cannot realize the control of optical foil crystal grains, and the improvement of specific volume and strength cannot be considered.
Disclosure of Invention
The invention aims to overcome the defects that the existing low-voltage anode aluminum optical foil annealing process for the aluminum electrolytic capacitor cannot realize the control of optical foil crystal grains and cannot improve the specific volume and strength of the corrosion foil, and provides the optical foil crystal grain control method which realizes the control of the crystal grain size and uniformity through the control of the vacuum degree and the heating rate in the annealing process so as to improve the specific volume and strength of the corrosion foil.
Another object of the present invention is to provide a method for producing an anode foil for an electrolytic capacitor.
It is still another object of the present invention to provide an anode foil for an electrolytic capacitor.
It is a further object of the present invention to provide the use of an anode foil for electrolytic capacitors for the preparation of aluminium electrolytic capacitors.
The above object of the present invention is achieved by the following technical scheme:
a method for controlling optical foil grains, comprising the steps of:
s1, placing an aluminum optical foil sample in an annealing furnace, vacuumizing the annealing furnace to a vacuum degree of 50-100 Pa, heating to 250 ℃, heating at a heating rate of 2-8 ℃/min, vacuumizing to less than or equal to 2Pa, preserving heat for 2-4h,
s2, maintaining the vacuum degree, heating to 420 ℃ at a heating rate of 1-2 ℃/min, continuously filling inert gas into the furnace at the vacuum degree, keeping the flow rate of 3-10L/min, and preserving the heat for 2-4h;
s3, cooling to 250 ℃ in a vacuum state, introducing air to normal pressure, cooling to 50-120 ℃ again at a cooling rate of 1-4 ℃/min, and discharging.
The following description is needed:
in step S1 of the present invention,
because of the high fault energy characteristic, the cold deformation pure aluminum can generate a strong recovery process in the heating process at 250 ℃, so that the dislocation density caused by cold deformation is greatly reduced, and the change of the dislocation density can greatly influence the driving force of recrystallization, thereby influencing the recrystallization behavior of the cold-rolled aluminum foil. Recrystallization is a nucleation and nucleation growth process, the driving force of which derives from the stored energy during processing deformation. After being heated at 250 ℃ in S1, a large amount of storage energy is released due to strong recovery action, so that the driving force of grain growth in the aluminum foil is reduced, the corresponding growth speed of grains is greatly reduced, and the size of recrystallized grains after high-temperature annealing is obviously smaller than that of a sample which is not subjected to recovery treatment.
The small and uniform size of the crystal grains can prevent uneven holes from being generated due to uneven crystal grains in the subsequent corrosion process, the specific volume is improved, and meanwhile, the bonding force between crystal boundaries is also ensured to be larger and more uniform, so that the strength (including tensile strength and bending strength) of the corrosion foil is improved, in addition, the process of preserving heat for 2-4 hours at the low temperature of 250 ℃ is adopted, the process of fully releasing water and oil gas of the foil is provided, and the adhesion of the foil caused by subsequent hydrogen re-infiltration and incomplete oil gas removal is avoided. By increasing the recrystallization temperature (420 ℃) and shortening the heat preservation time, the production time is greatly reduced, and the overgrowth of grains is avoided in a shorter time. The higher vacuum degree is favorable for smoothly discharging hydrogen in the foil, and the times of hydrogen evolution with high cost in the pure aluminum production process can be improved.
The optical foil grain control method of the invention controls the vacuum degree and the inert gas flow in the annealing process, firstly ensures the removal of water and oil in the foil coil at low temperature Duan Hengwen in the step S1, gives a recrystallization recovery energy process to the aluminum foil tissue structure, releases the energy accumulated by too high dislocation density caused by cold deformation in the aluminum foil rolling process, reduces the driving force of grain growth in the crystallization process, ensures uniform grain and avoids excessive grain and oversized individual size. After the recovery at low temperature is finished, the temperature in S2 is quickly raised to 420 ℃ to accelerate the recrystallization process of the crystal grains, so that the overlong heat preservation time is simplified, and the temperature rise and the heat preservation time are shorter, so that the crystal grains can be reasonably ensured not to be abnormally increased at high temperature, the production efficiency is improved, the aluminum foil tissue structure with proper size and uniform crystal grains is obtained, and the strength of the aluminum foil is ensured to be critically ensured after corrosion.
By the control method of the crystal grain of the optical foil, the annealing process for improving the production process of the optical foil can achieve the effects of improving the crystal structure of the optical foil, controlling the uniformity of the crystal grain and the size of the crystal grain, and further achieving the purpose of improving the strength of the aluminum foil after corrosion. In addition, the optical foil crystal grain control of the invention forcedly carries out secondary hydrogen evolution in a physical mode by adjusting the annealing temperature, so that aluminum core bubbles are not generated in the corrosion production process of the aluminum foil, thereby improving the strength of the aluminum foil.
The invention can lead the optical foil to have proper grain size and uniformity by controlling the annealing and recrystallization process, thereby being beneficial to the uniformity of the corrosion layer after corrosion processing.
Preferably, a high vacuum is drawn in S1 to 0.5 to 1Pa.
More preferably, a high vacuum is drawn in S1 to 4Pa.
In order to further better remove water and oil from the foil coil, the grain size and uniformity are better controlled, preferably the heating rate in S1 is 3-5 ℃/min, more preferably 4 ℃/min.
In a specific embodiment, in order to further obtain an aluminum foil structure with a proper size and uniform grains, the heating rate in S2 is preferably 1.4 ℃/min.
Preferably, the inert gas in S2 is 5-10L/min.
In a specific embodiment, the first cooling rate in S3 is a natural cooling rate maintained in a vacuum state, and the cooling rate is reduced to 250 ℃.
Preferably, the cooling rate in the step S3 is 2 ℃/min, and the furnace is discharged after the temperature is cooled to 50-120 ℃.
The invention also specifically protects a preparation method of the anode foil for the electrolytic capacitor, which comprises rough rolling, finish rolling, annealing, corrosion and formation of a high-purity aluminum ingot, wherein the annealing treatment adopts the control method of the optical foil crystal grain.
The invention also specifically protects the anode foil for the electrolytic capacitor, which is prepared by the preparation method.
The invention also specifically protects application of the anode foil for the electrolytic capacitor in preparing the aluminum electrolytic capacitor.
The optical foil grain control method can greatly optimize the annealing process of the anode foil for the electrolytic capacitor, prepare the optical foil with proper grain size and uniformity, is favorable for the uniformity of a corrosion layer after corrosion processing, remarkably improves the specific volume and strength of the anode foil, and can be widely applied to the field of aluminum electrolytic capacitors.
On the other hand, the invention also specifically protects an aluminum electrolytic capacitor, wherein the anode foil of the aluminum electrolytic capacitor is the anode foil for the electrolytic capacitor.
Compared with the prior art, the invention has the beneficial effects that:
according to the control method of the optical foil crystal grain, the vacuum degree and the inert gas flow of an annealing process are controlled, water and oil are removed at low temperature Duan Hengwen, energy is released, the driving force of crystal grain growth in the crystallization process is reduced, and then the crystal grain recrystallization is accelerated by rapid temperature rise, so that an aluminum foil tissue structure with proper size and uniform crystal grains is obtained, the specific volume is improved, the bonding force among crystal boundaries is ensured to be larger and more uniform, and the strength of the corrosion foil is improved. In addition, the optical foil crystal grain control of the invention forcedly carries out secondary hydrogen evolution in a physical mode by adjusting the annealing temperature, so that aluminum core bubbles are not generated in the corrosion production process of the aluminum foil, thereby improving the strength of the aluminum foil.
The grain control method of the optical foil can improve the specific volume of the final aluminum foil to (the specific volume of 21VF after the optical foil with 100 micrometers is corroded reaches 100 mu F/cm) 2 Above, promote aluminium foil intensity, tensile strength can reach 26N/CM, and bending strength can reach 100 returns.
Drawings
Fig. 1 is an EBSD grain diagram of the grain structure of the process optical foil of example 1.
Fig. 2 is an EBSD grain diagram of the grain structure of the annealing process photo-foil of comparative example 1.
Fig. 3 is a scanning electron microscope image of the aluminum foil of comparative example 5.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
Example 1
A method for controlling optical foil grains, comprising the steps of:
s1, placing a photo-foil sample in an annealing furnace, vacuumizing the annealing furnace to a vacuum degree of 100Pa, rapidly heating to 250 ℃, vacuumizing to 2Pa, and preserving heat for 2 hours at a heating rate of 4 ℃/min;
s2, maintaining the vacuum degree, rapidly heating to 420 ℃, keeping the heating rate at 1.4 ℃/min, continuously filling inert gas into the furnace at the vacuum degree, keeping the flow rate at 10L/min, and preserving the heat for 3 hours;
s3, naturally and slowly cooling to 250 ℃ in a vacuum state, filling air to maintain normal atmospheric pressure, then rapidly cooling to 100 ℃ and discharging, wherein the cooling rate is 2.5 ℃/min.
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
rough rolling, finish rolling, annealing, corrosion and formation of high-purity aluminum ingots,
wherein the annealing step was performed by using the optical foil grain control method of example 1 described above, respectively.
Example 2
A method for controlling optical foil grains, comprising the steps of:
s1, placing a photo-foil sample in an annealing furnace, vacuumizing the annealing furnace to a vacuum degree of 100Pa, rapidly heating to 250 ℃, vacuumizing to 1Pa, and preserving heat for 2 hours at a heating rate of 4 ℃/min;
s2, maintaining the vacuum degree, rapidly heating to 420 ℃, keeping the heating rate at 1.4 ℃/min, continuously filling inert gas into the furnace at the vacuum degree, keeping the flow rate at 10L/min, and preserving the heat for 3 hours;
s3, slowly cooling to 250 ℃, wherein the cooling rate is 0.65 ℃/min, charging air to maintain normal atmospheric pressure, then rapidly cooling to 100 ℃, discharging, and the cooling rate is 2.5 ℃/min.
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
rough rolling, finish rolling, annealing, corrosion and formation of high-purity aluminum ingots,
wherein the annealing step was performed by the optical foil grain control method of example 2 above, respectively.
Example 3
A method for controlling optical foil grains, comprising the steps of:
s1, placing a photo-foil sample in an annealing furnace, vacuumizing the annealing furnace to a vacuum degree of 100Pa, rapidly heating to 250 ℃, vacuumizing to 0.5Pa, and preserving heat for 2 hours at a heating rate of 4 ℃/min;
s2, maintaining the vacuum degree, rapidly heating to 420 ℃, keeping the heating rate at 1.4 ℃/min, continuously filling inert gas into the furnace at the vacuum degree, keeping the flow rate at 10L/min, and preserving the heat for 3 hours;
s3, slowly cooling to 250 ℃, wherein the cooling rate is 0.65 ℃/min, charging air to maintain normal atmospheric pressure, then rapidly cooling to 100 ℃, discharging, and the cooling rate is 2.5 ℃/min.
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
rough rolling, finish rolling, annealing, corrosion and formation of high-purity aluminum ingots,
wherein the annealing step was performed by the optical foil grain control method of example 3 above.
Example 4
A method for controlling optical foil grains, comprising the steps of:
s1, placing a photo-foil sample in an annealing furnace, vacuumizing the annealing furnace to a vacuum degree of 100Pa, rapidly heating to 250 ℃, vacuumizing to 1Pa, and preserving heat for 2 hours at a heating rate of 4 ℃/min;
s2, maintaining the vacuum degree, rapidly heating to 420 ℃, keeping the heating rate at 1.4 ℃/min, continuously filling inert gas into the furnace at the vacuum degree, keeping the flow at 5L/min, and preserving the heat for 3 hours;
s3, naturally and slowly cooling to 250 ℃ in a vacuum state, filling air to maintain normal atmospheric pressure, then rapidly cooling to 100 ℃ and discharging, wherein the cooling rate is 2.5 ℃/min.
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
rough rolling, finish rolling, annealing, corrosion and formation of high-purity aluminum ingots,
wherein the annealing step was performed by the optical foil grain control method of example 4 above, respectively.
Example 5
A method for controlling optical foil grains, comprising the steps of:
s1, placing a photo-foil sample in an annealing furnace, vacuumizing the annealing furnace to a vacuum degree of 100Pa, rapidly heating to 250 ℃, vacuumizing to 1Pa, and preserving heat for 2 hours at a heating rate of 8 ℃/min;
s2, maintaining the vacuum degree, rapidly heating to 420 ℃, keeping the heating rate at 1.4 ℃/min, continuously filling inert gas into the furnace at the vacuum degree, keeping the flow rate at 10L/min, and preserving the heat for 3 hours;
s3, naturally and slowly cooling to 250 ℃ in a vacuum state, filling air to maintain normal atmospheric pressure, then rapidly cooling to 100 ℃ and discharging, wherein the cooling rate is 2.5 ℃/min.
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
rough rolling, finish rolling, annealing, corrosion and formation of high-purity aluminum ingots,
wherein the annealing step was performed by the optical foil grain control method of example 5 above.
Example 6
A method for controlling optical foil grains, comprising the steps of:
s1, placing a photo-foil sample in an annealing furnace, vacuumizing the annealing furnace to a vacuum degree of 50Pa, rapidly heating to 250 ℃, vacuumizing to 1Pa, and preserving heat for 2 hours at a heating rate of 4 ℃/min;
s2, maintaining the vacuum degree, rapidly heating to 420 ℃, keeping the heating rate at 1.4 ℃/min, continuously filling inert gas into the furnace at the vacuum degree, keeping the flow rate at 10L/min, and preserving the heat for 3 hours;
s3, naturally and slowly cooling to 250 ℃ in a vacuum state, filling air to maintain normal atmospheric pressure, then rapidly cooling to 100 ℃ and discharging, wherein the cooling rate is 2.5 ℃/min.
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
rough rolling, finish rolling, annealing, corrosion and formation of high-purity aluminum ingots,
wherein the annealing step was performed by the optical foil grain control method of example 6 above.
Comparative example 1
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
cold rolling high-purity aluminium ingot, aluminium optical foil, annealing treatment, electric corrosion, formation and anode foil finished product
The annealing step adopts a conventional annealing scheme, the annealing is performed under the positive pressure of protective gas, the temperature is raised to 300 ℃, the heat is preserved for 15 hours, the temperature is lowered to 100 ℃, and the annealing is performed.
Comparative example 2
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
cold rolling high-purity aluminium ingot, aluminium optical foil, annealing treatment, electric corrosion, formation and anode foil finished product
Wherein, the annealing step adopts vacuum annealing, the temperature is raised to 420 ℃ under the vacuum degree of 2Pa, the heat is preserved for 2 hours, the temperature is reduced to 100 ℃, and the annealing is carried out.
Comparative example 3
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
cold rolling high-purity aluminium ingot, aluminium optical foil, annealing treatment, electric corrosion, formation and anode foil finished product
Wherein, the annealing step adopts vacuum annealing, the temperature is increased to 520 ℃ under the vacuum degree of 2Pa, the heat is preserved for 2 hours, the temperature is reduced to 100 ℃, and the annealing is carried out.
Comparative example 4
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
cold rolling high-purity aluminium ingot, aluminium optical foil, annealing treatment, electric corrosion, formation and anode foil finished product
Wherein, the annealing step adopts vacuum annealing, the temperature is raised to 300 ℃ under the vacuum degree of 2Pa, the heat is preserved for 15h, the temperature is reduced to 100 ℃, and the annealing is carried out.
Comparative example 5
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
cold rolling high-purity aluminium ingot, aluminium optical foil, annealing treatment, electric corrosion, formation and anode foil finished product
The annealing step is to adopt vacuum annealing, heat up to 250 ℃ under the vacuum degree of 2Pa, keep the temperature for 2 hours, quickly heat up to 500 ℃, keep the temperature for 2 hours, cool down to 100 ℃ and discharge from the furnace.
Comparative example 6
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
wherein the annealing step was vacuum annealing, which was substantially the same as in example 1 except that high vacuum was applied to 3Pa in S1.
Comparative example 7
The preparation method of the anode foil for the electrolytic capacitor specifically comprises the following steps:
wherein the annealing step was vacuum annealing, which was substantially the same as example 1, except that S1 was heated to 250℃at a heating rate of 10℃per minute.
Result detection
10 surface texture test, specific test, was performed on the grain structure of the aluminum foil before and after annealing in example 1
The measuring method comprises the following steps: and (3) curing the annealed optical foil by using epoxy resin, grinding and polishing a detection surface, and then performing EBSD detection by using a scanning electron microscope.
The test results are shown in Table 1 below:
table 1.
Wherein the strength of the aluminum foil is better than 90 times of bending strength, the qualified aluminum foil is 75-89 times of bending strength, and the inferior aluminum foil is less than 75 times of bending strength.
The results of the grain structure detection of the aluminum foils of other examples 1 to 6 are basically the same as those of example 1, the grain size is uniform, the annealing time period is long, the strength of the aluminum foil is excellent, and other adverse phenomena are avoided.
Fig. 1 is a graph of EBSD grains after annealing treatment by the photo-foil grain control method of example 1, and it can be seen that uniform and properly sized grains are obtained.
Fig. 2 is an EBSD grain diagram of an aluminum foil after annealing treatment by the photo-foil grain control method of comparative example 1, and it can be seen that the grains are not uniform in size and the annealing time is long.
In addition, fig. 3 is a scanning electron microscope image of the aluminum foil of comparative example 5, and it can be seen from the image that if the vacuum is insufficient, the moisture is not removed, the hydrogen gas is accumulated and exploded in the foil core layer, so that the local air holes appear, and the strength is affected.
The specific volume and strength of the aluminum foils of the above examples and comparative examples of the present invention were measured as follows:
specific volume: after the optical foil is corroded and formed, specific volume detection is carried out under the test voltage of 21VF, and the unit is mu F/cm 2 。
Tensile strength: the strip foil of 10 x 1 cm was subjected to tensile testing in N/cm using a tensile machine.
Bending strength: bending test is carried out by a bending machine, wherein the sample is 10-1 cm, and the unit is: and (5) returning.
The specific detection results are shown in the following table 2:
table 2.
| Sequence number | Specific volume | Tensile Strength | Bending strength |
| Example 1 | 103 | 26 | 95 |
| Example 2 | 105 | 26 | 105 |
| Example 3 | 103 | 26 | 95 |
| Example 4 | 105 | 26 | 105 |
| Example 5 | 100 | 26 | 82 |
| Example 6 | 105 | 26 | 103 |
| Comparative example 6 | 103 | 26 | 65 |
| Comparative example 7 | 95 | 26 | 75 |
As can be seen from Table 2 above, the specific volume of the aluminum foil of the present invention can reach 100. Mu.F/cm 2 The aluminum foil has good strength, the tensile strength is 26N/cm, and the bending strength can be excellent.
In comparative example 6, the degree of vacuum of the high vacuum is insufficient, the strength of the aluminum foil is obviously affected, the strength of the aluminum foil is poor, and the bending strength is lower than 75 times.
In comparative example 7, the heating rate to 250 c was too high, and the specific volume and strength of the aluminum foil were both lowered. It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (10)
1. The optical foil grain control method is characterized by comprising the following steps:
s1, placing an aluminum optical foil sample in an annealing furnace, vacuumizing the annealing furnace to a vacuum degree of 50-100 Pa, heating to 250 ℃, heating at a heating rate of 2-8 ℃/min, vacuumizing to 0.5-2 Pa, preserving heat for 2-4h,
s2, maintaining the vacuum degree, heating to 420 ℃ at a heating rate of 1-2 ℃/min, continuously filling inert gas into the furnace at the vacuum degree, keeping the flow rate of 3-10L/min, and preserving the heat for 2-4h;
s3, cooling to 250 ℃ in a vacuum state, introducing air to normal pressure, cooling to 50-120 ℃ again at a cooling rate of 1-4 ℃/min, and discharging.
2. The method of controlling a photo-foil grain according to claim 1, wherein the high vacuum is applied to 0.5 to 1Pa in S1.
3. The method of controlling a photo-foil grain according to claim 1, wherein the high vacuum is applied to 1Pa in S1.
4. The method of controlling a photo-foil grain according to claim 1, wherein the temperature rise rate in S1 is 3 to 5 ℃/min.
5. The method of controlling a photo-foil grain according to claim 1, wherein the temperature rise rate in S1 is 4 ℃/min.
6. The method of controlling a photo-foil grain according to claim 1, wherein the inert gas in S2 is 5 to 10L/min.
7. A method for preparing an anode foil for an electrolytic capacitor, comprising rough rolling, finish rolling, annealing, corrosion and formation of a high-purity aluminum ingot, wherein the annealing treatment is performed by the optical foil grain control method according to any one of claims 1 to 6.
8. An anode foil for electrolytic capacitors produced by the production method of claim 7.
9. Use of the anode foil for electrolytic capacitors as claimed in claim 8 for the production of aluminum electrolytic capacitors.
10. An aluminum electrolytic capacitor, wherein the anode foil of the aluminum electrolytic capacitor is the anode foil for an electrolytic capacitor according to claim 8.
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