A multi-stage formation method and system for preparing an aluminum electrolytic capacitor anode foil

Abstract

The application discloses a multistage formation method and system for preparing an aluminum electrolytic capacitor anode foil, the formation system comprises first to seventh formation tanks for performing first to seventh formation treatments and first to fourth eighth formation tanks for performing first to fourth eighth formation treatments, and each formation tank is provided with a plurality of V-shaped conveying devices formed by V-shaped guide rollers, and the contact time of the foil material on the V-shaped conveying device with the tank liquid in the tank is 80-120s. The application can realize eight or more formation, further improves the processing speed, and can simultaneously solve the problems of oxide film defects caused by high speed and the like, improves the production efficiency, reduces the production cost, and the obtained formation foil has a high-quality dielectric layer, high capacity and low leakage current.

Description

Technical Field

[0001] This invention relates to the technical field of methods for preparing anode foil for aluminum electrolytic capacitors, and particularly to the technical field of multi-stage formation methods for anode foil. Background Technology

[0002] The anode foil is one of the key components that limits the performance of aluminum electrolytic capacitors. With the development of science and technology and the electronics industry, the market has put forward higher performance requirements for aluminum electrolytic capacitors, and miniaturization, long life and high capacity have become development trends. The production of anode foil by forming a dense oxide film on the etched foil using a multi-stage formation process to obtain a dielectric layer with a specific voltage resistance has become the mainstream formation process for aluminum electrolytic capacitors.

[0003] Compared to formation processes with fewer formation stages, multi-stage formation can not only obtain an excellent dielectric layer and anode foil with long life, high capacity, and low leakage current, but also reduce the current loss of each formation stage by increasing the formation speed and obtaining an excellent oxide film, thus greatly saving production costs.

[0004] However, in actual production, while increasing the number of formation stages increases the production speed, it also shortens the reaction time between the aluminum foil and the bath solution. This results in more defects in the oxide film generated in each formation stage, which can easily cause flashover in subsequent formation stages, damaging the dielectric layer on the foil and reducing the quality of the resulting oxide film, thus lowering the performance of the final product. At the same time, it also increases production costs due to the large amount of electrical energy being converted into heat. To improve this problem, the production speed can be reduced, but this would negate the advantages of multi-stage formation itself.

[0005] Furthermore, as shown in existing patent documents such as CN114525565A, CN103227053B, CN108155016B, and CN112768245A, which propose six or more formation processes, although they have made great progress in terms of processing speed, leakage current, and capacity of products, many of these methods equate repair treatment with one stage in multi-stage formation. The actual number of formation stages is still low, and multiple formation stages use the same formation parameters, which cannot achieve the effect of step-by-step voltage increase and cannot fully utilize the advantages of multi-stage formation. The resulting products still have defects such as large leakage current, low production efficiency, and long process time, and cannot efficiently and cost-effectively produce anode foil that meets high-quality requirements. Summary of the Invention

[0006] In view of the shortcomings of the prior art, the purpose of this invention is to propose a new multi-stage formation system and method for preparing aluminum electrolytic capacitor anode foil. This system or method can achieve more than eight stages of formation, further improve the processing speed, and simultaneously solve problems such as oxide film defects caused by high speed, thereby improving production efficiency, reducing production costs, and the resulting formed foil has a high-quality dielectric layer with high capacity and low leakage current.

[0007] The technical solution of the present invention is as follows:

[0008] A multi-stage formation method for preparing anode foil for aluminum electrolytic capacitors includes: sequentially subjecting the aluminum etched foil to hydration treatment via a continuously conveying V-shaped conveyor; a first-stage formation treatment in a first treatment solution; a second-stage formation treatment in a second treatment solution; a third-stage formation treatment in a third treatment solution; a fourth-stage formation treatment in a fourth treatment solution; a fifth-stage formation treatment in a fifth treatment solution; a sixth-stage formation treatment in a sixth treatment solution; a seventh-stage formation treatment in a seventh treatment solution; a first-eighth-stage formation treatment in a first-eighth-stage treatment solution; and a second-eighth-stage formation treatment in a second-eighth-stage treatment solution. The formation processes include a third-eighth-stage formation process performed in a third-eighth-stage processing solution and a fourth-eighth-stage formation process performed in a fourth-eighth-stage processing solution; wherein the formation voltages for the first-stage, second-stage, third-stage, fourth-stage, fifth-stage, sixth-stage, seventh-stage, first-eighth-stage, second-eighth-stage, third-eighth-stage, and fourth-eighth-stage formation processes are 100V, 180V, 260V, 340V, 410V, 480V, 510V, 530V, 530V, 530V, and 530V, respectively, and the formation currents are 30-50mA / cm², respectively. 2 30-40mA / cm 2 30-45mA / cm 2 30-35mA / cm 2 26-32mA / cm 2 25-30mA / cm 2 25-30mA / cm 2 25-30mA / cm 2 25-30mA / cm 2 25-30mA / cm 2 25-30mA / cm 2The V-shaped conveyor consists of three guide rollers arranged in a V-shape. The contact time between the foil material on each V-shaped conveyor and each treatment liquid is 80-120 seconds. The number of V-shaped conveyors used in the hydration treatment, primary treatment, secondary formation treatment, tertiary formation treatment, quaternary formation treatment, quinary formation treatment, sixth formation treatment, seventh formation treatment, first octet formation treatment, second octet formation treatment, third octet formation treatment, and fourth octet formation treatment are 6-8, 2-4, 2-4, 2-4, 2-4, 2-4, 2-4, 4-6, 6-7, 3-4, 2-3, and 1-2, respectively.

[0009] According to some preferred embodiments of the present invention, the three V-shaped guide rollers include two equally spaced drive rollers located at the top and a bottom roller located in the middle below the two drive rollers.

[0010] According to some preferred embodiments of the present invention, the multi-stage formation method further includes: a first phosphoric acid treatment performed by the V-shaped conveyor after the first eight-stage formation treatment, a second phosphoric acid treatment after the second eight-stage formation treatment, and a post-treatment after the fourth eight-stage formation treatment.

[0011] According to some preferred embodiments of the present invention, the number of the V-shaped conveyors used in the first phosphoric acid treatment, the second phosphoric acid treatment, and the post-treatment are 1, 3, and 2, respectively.

[0012] According to some preferred embodiments of the present invention, the first treatment solution comprises: a mixed aqueous solution of ammonium adipate (3-5 g / L), boric acid (8-10 g / L), ammonium azelate (3-5 g / L), sodium hypophosphite (1-2 g / L), and citric acid (4-5 g / L); the second treatment solution comprises: a mixed aqueous solution of ammonium adipate (2-4 g / L), boric acid (8-10 g / L), ammonium azelate (2.5-4 g / L), sodium hypophosphite (1-2 g / L), and citric acid (4-5 g / L); the third treatment solution comprises: a mixed aqueous solution of boric acid (20-40 g / L), citric acid (2-6 g / L), and ammonium azelate (5-7 g / L); and the fourth treatment solution comprises: a mixed aqueous solution of ammonium azelate (50-60 g / L). The fifth treatment solution comprises a mixed aqueous solution of boric acid, citric acid, and ammonium azelate at a concentration of 50-60 g / L; the sixth treatment solution comprises a mixed aqueous solution of boric acid and ammonium pentaborate at a concentration of 50-60 g / L; the seventh treatment solution comprises a mixed aqueous solution of boric acid and ammonium pentaborate at a concentration of 50-60 g / L; the first, second, third, and fourth eighth-stage treatment solutions all comprise a mixed aqueous solution of boric acid and ammonium pentaborate at a concentration of 50-60 g / L.

[0013] According to some preferred embodiments of the present invention, the multi-stage formation method specifically includes:

[0014] The foil material is conveyed through the V-shaped conveyor, and the following steps are performed sequentially:

[0015] (1) Boil aluminum etched foil in pure water at 92-98°C to obtain hydrated foil;

[0016] (2) The hydrated foil is subjected to a first-stage formation treatment in a first-stage treatment solution to obtain a first-stage treated foil; the first-stage treatment solution comprises: a mixed aqueous solution of ammonium adipate (3-5 g / L), boric acid (8-10 g / L), ammonium azelate (3-5 g / L), sodium hypophosphite (1-2 g / L), and citric acid (4-5 g / L); during the formation treatment, the temperature of the first-stage treatment solution is controlled at 80-90°C, the formation voltage is 100 V, and the formation current is 30-50 mA / cm. 2 ;

[0017] (3) The primary processed foil is subjected to a secondary formation process in a second processing solution to obtain a secondary processed foil; the second processing solution comprises: a mixed aqueous solution of ammonium adipate (2-4 g / L), boric acid (8-10 g / L), ammonium azelaate (2.5-4 g / L), sodium hypophosphite (1-2 g / L), and citric acid (4-5 g / L). During the formation process, the temperature of the second processing solution is controlled at 85±5℃, the formation voltage is 180V, and the formation current is 30-40mA / cm. 2 ;

[0018] (4) The secondary-treated foil is sprayed and washed with water, and then subjected to a tertiary formation treatment in a third treatment solution to obtain a tertiary-treated foil; the third treatment solution comprises a mixed aqueous solution of boric acid (20-40 g / L), citric acid (2-6 g / L), and ammonium azelate (5-7 g / L). During the formation treatment, the temperature of the third treatment solution is controlled at 85±5℃, the formation voltage is 260V, and the formation current is 30-45mA / cm. 2 ;

[0019] (5) The three-stage treated foil is immersed and washed with water, and then subjected to a four-stage formation treatment in a fourth treatment solution to obtain a four-stage treated foil; the fourth treatment solution includes a mixed aqueous solution of boric acid (50-60 g / L), citric acid (2-6 g / L), and ammonium azelate (4-6 g / L). During the formation treatment, the temperature of the fourth treatment solution is controlled at 85±5℃, the formation voltage is 340V, and the formation current is 30-35mA / cm. 2 ;

[0020] (6) The fourth-stage treated foil is sprayed and washed with water, and then subjected to a fifth-stage formation treatment in a fifth treatment solution to obtain a fifth-stage treated foil. The fifth treatment solution comprises a mixed aqueous solution of boric acid (50-60 g / L), citric acid (2-6 g / L), and ammonium azelate (4-6 g / L). During the formation treatment, the temperature of the fourth-stage treated solution is controlled at 85±5℃, the formation voltage is 410V, and the formation current is 26-32mA / cm. 2 ;

[0021] (7) The fifth-stage treated foil is sprayed and washed with water, and then subjected to a sixth-stage formation process in a sixth-stage treatment solution to obtain a sixth-stage treated foil. The sixth-stage treatment solution comprises a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation process, the temperature of the fifth-stage treatment solution is controlled at 85±5℃, the formation voltage is 480V, and the formation current is 25-30mA / cm. 2 ;

[0022] (8) The sixth-stage treated foil is sprayed and washed with water, and then subjected to a seventh-stage formation process in a seventh-stage treatment solution to obtain a seventh-stage treated foil. The seventh-stage treatment solution comprises a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation process, the temperature of the fifth-stage treatment solution is controlled at 85±5℃, the formation voltage is 510V, and the formation current is 25-30 mA / cm. 2 ;

[0023] (9) The seventh-stage treated foil is immersed and washed with water, and then subjected to a first-eighth-stage formation treatment in a first-eighth-stage treatment solution to obtain a first-eighth-stage treated foil. The first-eighth-stage treatment solution comprises a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation treatment, the temperature of the first-eighth-stage treatment solution is controlled at 85±5℃, the formation voltage is 530V, and the formation current is 25-30mA / cm. 2 ;

[0024] (10) The first eighth-level treated foil is washed with water and then subjected to phosphoric acid treatment at 55±5℃ in the first phosphoric acid solution. The treated foil is washed with water and then calcined at 520-550℃ for 2 minutes to obtain the first heat-treated foil. The mass percentage concentration of the first phosphoric acid solution is 5%.

[0025] (11) The first heat-treated foil is subjected to a second-eighth-stage formation process in a second-eighth-stage processing solution to obtain a second-eighth-stage treated foil. The second-eighth-stage processing solution comprises a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation process, the temperature of the second-eighth-stage processing solution is controlled at 85±5℃, the formation voltage is 530 V, and the formation current is 25-30 mA / cm. 2 ;

[0026] (12) After washing the second eighth-level treated foil with water, immerse it in the second phosphoric acid solution for 150-180s, and then wash it with water to obtain a water-washed foil. The mass percentage concentration of the second phosphoric acid solution is 10%.

[0027] (13) The washed foil is subjected to a third-eighth-stage formation treatment in a third-eighth-stage treatment solution to obtain a third-eighth-stage treated foil. The third-eighth-stage treatment solution comprises a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation treatment, the temperature of the third-eighth-stage treatment solution is controlled at 85±5℃, the formation voltage is 530 V, and the formation current is 25-30 mA / cm. 2 ;

[0028] (14) The third grade eight-stage treated foil is washed with water and then calcined at 420-500℃ for 2 minutes to obtain the second heat-treated foil;

[0029] (15) The second heat-treated foil is subjected to a fourth-eighth-stage formation treatment in a fourth-eighth-stage processing solution to obtain a fourth-eighth-stage treated foil. The fourth-eighth-stage processing solution comprises a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation treatment, the temperature of the fourth-eighth-stage processing solution is controlled at 85±5℃, the formation voltage is 530 V, and the formation current is 25-30 mA / cm. 2 ;

[0030] (16) The fourth and eighth grade processed foil is washed with water and then immersed in a 6 g / L ammonium dihydrogen phosphate solution, followed by washing and drying to obtain the chemically processed foil.

[0031] According to some preferred embodiments of the present invention, the secondary formation process, tertiary formation process, quaternary formation process, quinary formation process, sixth formation process, seventh formation process, first octet formation process, second octet formation process, third octet formation process, and fourth octet formation process are all achieved by liquid power supply device.

[0032] According to some preferred embodiments of the present invention, the primary formation process is achieved by powering a silver roller, which means that the silver roller is powered by a silver conductive roller that is connected to the V-shaped conveyor and connected to a power source.

[0033] This invention further provides a formation system for implementing the above-mentioned multi-stage formation method, comprising: a hydration tank, a first-stage formation tank, a second-stage formation tank, a third-stage formation tank, a fourth-stage formation tank, a fifth-stage formation tank, a sixth-stage formation tank, a seventh-stage formation tank, a first-eighth-stage formation tank, a second-eighth-stage formation tank, a third-eighth-stage formation tank, and a fourth-eighth-stage formation tank, respectively, for performing the hydration treatment, first-stage formation treatment, second-stage formation treatment, third-eighth-stage formation treatment, and fourth-eighth-stage formation treatment; and each formation tank is provided with a plurality of V-shaped conveyors, wherein the V-shaped conveyors consist of three V-shaped... The V-shaped guide rollers are arranged in a specific configuration, including two equally spaced drive rollers at the top and a bottom roller located in the middle below the two drive rollers. The contact time between the foil material on the V-shaped conveyor and the bath liquid in the tank is 80-120 seconds. The number of V-shaped conveyors in the hydration tank, primary formation tank, secondary formation tank, tertiary formation tank, quaternary formation tank, quinary formation tank, sixth formation tank, seventh formation tank, first octave formation tank, second octave formation tank, third octave formation tank, and fourth octave formation tank are 6-8, 2-4, 2-4, 2-4, 2-4, 2-4, 2-4, 4-6, 6-7, 3-4, 2-3, and 1-2, respectively.

[0034] According to some preferred embodiments of the present invention, the formation system further includes: a first phosphoric acid tank located between the first eight-stage formation tank and the second eight-stage formation tank, a second phosphoric acid tank located between the second eight-stage formation tank and the third eight-stage formation tank, and a post-treatment tank located after the fourth eight-stage formation tank; a plurality of the V-shaped conveyors are provided in the hydration tank, the first phosphoric acid tank, the second phosphoric acid tank, and the post-treatment tank.

[0035] According to some preferred embodiments of the present invention, the number of V-shaped conveyors provided in the first phosphate tank, the second phosphate tank, and the post-treatment tank are 1, 3, and 2, respectively.

[0036] According to some preferred embodiments of the present invention, the formation system further includes: a first liquid-feed power supply device for supplying power to the secondary formation tank and the tertiary formation tank; a second liquid-feed power supply device for supplying power to the quaternary formation tank and the quinary formation tank; a third liquid-feed power supply device for supplying power to the sixth formation tank and the seventh formation tank; and a fourth liquid-feed power supply device for supplying power to the first octave formation tank, the second octave formation tank, the third octave formation tank, and the fourth octave formation tank.

[0037] According to some preferred embodiments of the present invention, the formation system further includes: a silver conductive roller located in front of the hydration tank and drivenly connected to a V-shaped conveyor in the hydration tank, the silver conductive roller being connected to a power source.

[0038] Through this preferred embodiment, the primary formation process of the present invention can be directly achieved by powering the silver roller.

[0039] According to some preferred embodiments of the present invention, each liquid-fed power supply device uses an ammonium adipate solution with a conductivity of 35,000 as the conductive liquid.

[0040] The formation system of the present invention is equipped with multiple conveying components capable of V-shaped conveying in each formation tank, which can increase and precisely control the reaction time between the formation tank liquid and the aluminum foil in each stage, and solve the problems of oxide film defects, flash fire, energy waste, low product specific volume, and large leakage current caused by high speed in multi-stage formation processes.

[0041] In some specific embodiments, this invention employs a power supply mode of silver rollers and a four-stage liquid feed system. Under low voltage, power is supplied via the silver rollers, leveraging their advantages of rapid and high conductivity at low voltages. Under high voltage, power is supplied via the liquid feed system. This four-stage liquid feed system maximizes the cooling effect of the liquid feed system at high voltages, saving energy while reducing issues such as flashover. This not only reduces tank pressure drop but also helps to distribute unnecessary and ineffective power generated by ion conduction in the liquid feed system.

[0042] The formation system or method of the present invention can achieve eight-stage formation. Compared with other multi-stage formation methods, it has a faster speed and higher production efficiency. It achieves step-by-step pressure increase at each stage, and the conductivity of each formation tank is also increased accordingly. The dense oxide film is formed by step-by-step stacking, and the produced anode foil has a high-quality dielectric layer. Attached Figure Description

[0043] Figure 1 This is a schematic diagram of a foil material conveying method for a single V-shaped conveyor.

[0044] Figure 2 This is a schematic diagram of a processing tank structure containing a single V-shaped conveyor used in the formation system of the present invention.

[0045] Figure 3 This is a schematic diagram of a processing tank structure containing multiple V-shaped conveyors specifically used in the formation system of the present invention.

[0046] Figure 4 This is a schematic diagram of the multi-stage formation system of the present invention.

[0047] Figure 5 This is a microscopic morphology diagram of the oxide film obtained in Example 1 of the present invention. Detailed Implementation

[0048] The present invention will now be described in detail with reference to embodiments and accompanying drawings. However, it should be understood that the embodiments and drawings are for illustrative purposes only and do not constitute any limitation on the scope of protection of the present invention. All reasonable modifications and combinations included within the inventive spirit of the present invention fall within the scope of protection of the present invention.

[0049] Example 1

[0050] See attached document Figure 1-3 The V-shaped conveyor used in this embodiment includes two equally arranged drive rollers 1-1 and 1-2 at the top and a bottom roller 2 located in the middle below the two drive rollers. These rollers are individually or in combination and placed in the tank body 3 of each processing tank. Each processing tank is filled with processing liquid (i.e., tank liquid). The contact time between the foil material B on the V-shaped conveyor and each processing liquid is the time from when the foil material B is immersed in the processing liquid to when it comes out of the processing liquid. In the formation process of this invention, the V-shaped conveyor works continuously. Therefore, the contact time between the foil material B and each processing liquid is a continuous time, rather than a periodic time period (i.e., during the preparation, the foil material conveying will not be stopped to allow it to remain still and immersed in the processing liquid in order to meet the time requirements).

[0051] Meanwhile, the formation system used in this embodiment includes two power supply methods: silver roller power supply and liquid-feed power supply. Silver roller power supply is achieved through a silver conductive roller connected to a power source, while liquid-feed power supply is achieved through a liquid-feed power supply device. Each liquid-feed power supply device uses an ammonium adipate solution with a conductivity of 35,000 for conduction.

[0052] In this embodiment, the contact time between the aluminum foil and the bath liquid under a single V-shaped conveyor is 100s.

[0053] Further, refer to the appendix. Figure 4 The formation process in this embodiment includes:

[0054] (1) Hydration treatment: The aluminum etched foil raw material is conveyed to the hydration tank through a silver conductive roller. The hydration tank is equipped with 7 V-shaped conveyors. The tank liquid is pure water, so that the aluminum etched foil is boiled in pure water at 92-98℃.

[0055] (2) Primary Formation: The hydrated aluminum foil is immersed in primary formation tank F1. Tank F1 is equipped with three V-shaped conveyors. The tank solution consists of a mixed aqueous solution of 3-5 g / L ammonium adipate, 8-10 g / L boric acid, 3-5 g / L ammonium azelaate, 1-2 g / L sodium hypophosphite, and 4-5 g / L citric acid. The tank solution temperature is 80-90℃, the formation tank voltage is 100V, and the formation tank current is 40 mA / cm². 2 It adopts a silver roller power supply method;

[0056] (3) Secondary Formation: The aluminum foil that has completed the primary formation is immersed in the secondary formation tank F2. F2 consists of three V-shaped conveyors. The tank solution includes a mixed aqueous solution of 2-4 g / L ammonium adipate, 8-10 g / L boric acid, 2.5-4 g / L ammonium azelaate, 1-2 g / L sodium hypophosphite, and 4-5 g / L citric acid. The tank solution temperature is 85±5℃, the voltage is 180V, and the current density is 36 mA / cm². 2 ;

[0057] (4) First-stage spray washing: The aluminum foil that has completed the second-stage formation is sprayed and washed in the first-stage spray washing tray. The washing tray is not equipped with V-shaped conveyor parts. The foil is cleaned by immersion in pure water.

[0058] (5) Tertiary Formation: The aluminum foil that has completed the first-stage water washing is placed into the tertiary formation tank F3. F3 includes three V-shaped conveyors. The tank solution consists of a mixed aqueous solution of 20-40 g / L boric acid, 2-6 g / L citric acid, and 5-7 g / L ammonium azelate. The tank solution temperature is controlled at 85±5℃, the voltage is 260V, and the current density is 34 mA / cm². 2 ;

[0059] (6) Secondary spray washing: The aluminum foil that has completed the tertiary formation is sprayed and cleaned in the secondary spray washing tray in the same way as the primary washing.

[0060] (7) Power supply of primary liquid power supply device: power supply to secondary formation tank F2 and tertiary formation tank F3 through the liquid power supply mode of primary liquid power supply device KD1. The specific power supply method is: using ammonium adipate solution with a conductivity of 35000 as the conductive liquid, conduction to the foil to form current loops with F2 and F3 respectively.

[0061] (8) First-stage water washing: Immerse the foil from step (7) into the first-stage water washing tank and wash it in pure water;

[0062] (9) Fourth-stage formation: The aluminum foil that has completed the first-stage water washing is immersed in the fourth-stage formation tank F4. F4 includes three V-shaped conveyors. The tank solution consists of a mixed aqueous solution of 50-60 g / L boric acid, 2-6 g / L citric acid, and 4-6 g / L ammonium azelate. The tank solution temperature is controlled at 85±5℃, the voltage is 340V, and the current density is 32mA / cm². 2 ;

[0063] (10) Three-stage spray washing: The aluminum foil that has completed the fourth stage of formation is sprayed and cleaned in the three-stage spray washing tray, which is the same as the first-stage spray washing method.

[0064] (11) Fifth-stage formation: The aluminum foil that has completed the third-stage spray washing is immersed in the fifth-stage formation tank F5. F5 includes three V-shaped conveyors. The tank solution consists of a mixed aqueous solution of 50-60 g / L boric acid, 4-6 g / L ammonium azelate, and 2-6 g / L citric acid. The tank solution temperature is controlled at 85±5℃, the voltage is 410V, and the current density is 30 mA / cm². 2 ;

[0065] (12) Fourth-stage spray washing: The aluminum foil that has completed the fifth-stage formation is sprayed and cleaned in the fourth-stage spray washing tray, which is the same as the first-stage spray washing method.

[0066] (13) Secondary liquid power supply: The liquid power supply mode of the second liquid power supply device KD2 is to supply power to the fourth-stage formation tank F4 and the fifth-stage formation tank F5. The conductive liquid is an ammonium adipate solution with a conductivity of 35000.

[0067] (14) Secondary water washing: Immerse the foil from step (13) into the secondary water washing tank and wash it in pure water;

[0068] (15) Sixth-stage formation: The aluminum foil that has completed the second-stage water washing is immersed in the sixth-stage formation tank F6. F6 includes three V-shaped conveyors. The tank solution consists of a mixed aqueous solution of 50-60 g / L boric acid and 3-5 g / L ammonium pentaborate. The tank solution temperature is controlled at 85±5℃, the voltage is 480V, and the current density is 28 mA / cm². 2 ;

[0069] (16) Five-stage spray washing: The aluminum foil that has completed the sixth-stage formation is sprayed and cleaned in the five-stage spray washing tray, using the same method as the first-stage spray washing.

[0070] (17) Seven-stage formation: The aluminum foil that has completed five-stage spray washing is immersed in the seven-stage formation tank F7. F7 includes five V-shaped conveyors. The tank solution consists of a mixed aqueous solution of 50-60 g / L boric acid and 3-5 g / L ammonium pentaborate. The tank solution temperature is controlled at 85±5℃, the voltage is 510V, and the current density is 28 mA / cm². 2 ;

[0071] (18) Three-stage liquid power supply: The liquid power supply mode through the third liquid power supply device KD3 is the sixth-stage formation tank F6 and the seventh-stage formation tank F7. The conductive liquid is an ammonium adipate solution with a conductivity of 35000.

[0072] (19) Three-stage water washing: Immerse the foil from step (18) into a three-stage water washing tank and wash it in pure water;

[0073] (20) First Eighth-Stage Formation: The aluminum foil that has completed the three-stage water washing process is immersed in the first eighth-stage formation tank F8-1. F8-1 includes 7 V-shaped conveyors. The tank solution consists of a mixed aqueous solution of 50-60 g / L boric acid and 3-5 g / L ammonium pentaborate. The tank solution temperature is controlled at 85±5℃, the voltage is 530V, and the current density is 28mA / cm. 2 ;

[0074] (21) Four-stage water washing: The foil that has completed the first eight-stage formation is immersed in the four-stage water washing tank and washed in pure water;

[0075] (22) First phosphoric acid treatment: The foil that has been washed in the four-stage water washing tank is placed into the first phosphoric acid treatment tank. The first phosphoric acid treatment tank includes a V-shaped conveyor. The tank solution is a phosphoric acid solution with a mass percentage of 5%. The temperature of the tank solution is controlled at 55±5℃.

[0076] (23) Five-stage water washing: The foil that has completed the first phosphoric acid treatment is immersed in the five-stage water washing tank and washed in pure water;

[0077] (24) First heat treatment: Place the foil that has been washed in the five-stage water washing tank into a baking furnace and bake it at 520-550℃ for 2 minutes;

[0078] (25) Second-stage formation: The foil that has completed the first heat treatment is immersed in the second-stage formation tank F8-2. F8-2 includes four V-shaped conveyors. The bath solution includes a mixed aqueous solution of 50-60 g / L boric acid and 3-5 g / L ammonium pentaborate. The bath solution temperature is controlled at 85±5℃, the voltage is 530V, and the current density is 28mA / cm. 2 ;

[0079] (26) Six-stage water washing: The foil that has completed the second eight-stage formation is immersed in the six-stage water washing tank and washed in pure water;

[0080] (27) Second phosphoric acid treatment: The foil that has been washed in the six-stage water washing tank is immersed in phosphoric acid with a mass percentage of 10% for 150-180 seconds. The second phosphoric acid treatment tank includes 3 V-shaped conveyors.

[0081] (28) Seven-stage water washing: The foil that has completed the second phosphoric acid treatment is immersed in a seven-stage water washing tank and washed in pure water;

[0082] (29) Third-stage formation: The aluminum foil that has completed the seventh-stage water washing is immersed in the third-stage formation tank F8-3. F8-3 includes three V-shaped conveyors. The tank solution consists of a mixed aqueous solution of 50-60 g / L boric acid and 3-5 g / L ammonium pentaborate. The tank solution temperature is controlled at 85±5℃, the voltage is 530V, and the current density is 28mA / cm. 2 ;

[0083] (30) Eight-stage water washing: The foil that has completed the third eight-stage formation process is immersed in the eight-stage water washing tank and washed in pure water;

[0084] (31) Second heat treatment: After cleaning the foil that has been washed in the eight-stage water washing tank, put it into the baking furnace and bake it at 420-500℃ for 2 minutes.

[0085] (32) Fourth-stage formation: The aluminum foil that has undergone the second heat treatment is immersed in the fourth-stage formation tank F8-4. F8-4 consists of two V-shaped conveyors. The bath solution consists of a mixed aqueous solution of 50-60 g / L boric acid and 3-5 g / L ammonium pentaborate. The bath solution temperature is controlled at 85±5℃, the voltage is 530V, and the current density is 28mA / cm. 2 ;

[0086] (33) Four-stage liquid power supply: The liquid power supply mode of the fourth liquid power supply device KD4 supplies power to the first eight-stage formation tank F8-1, the second eight-stage formation tank F8-2, the third eight-stage formation tank F8-3, and the fourth eight-stage formation tank F8-4. The conductive liquid is an ammonium adipate solution with a conductivity of 35000.

[0087] (34) Nine-stage water washing: Immerse the foil after completing step (33) into the nine-stage water washing tank and wash it in pure water;

[0088] (35) Post-treatment: The foil that has been washed in the nine-stage water washing tank is immersed in an ammonium dihydrogen phosphate aqueous solution with a mass concentration of 6 g / L for wetting treatment. The post-treatment tank consists of two V-shaped conveyor components.

[0089] (36) Ten-stage water washing: Immerse the finished foil in a ten-stage water washing tank and wash it in pure water;

[0090] (37) Drying: Place the foil that has been washed in the ten-stage water washing tank into a drying oven and dry it at 200°C to obtain chemical foil.

[0091] Example 2

[0092] The same preparation process as in Example 1 was used to prepare the chemical foil, except that the number of V-shaped conveyors in the hydration tank and the primary formation tank F1 was reduced. Specifically, only 6 V-shaped conveyors were set in the hydration tank, and only 2 V-shaped conveyors were set in the primary formation tank F1. At the same time, the formation current in F1 was adjusted to 50 mA / cm. 2 .

[0093] Example 3

[0094] The same preparation process as in Example 1 was used to prepare the formation foil, except that the number of V-shaped conveyors in the secondary-to-seventh stage formation tanks F2-F7 was reduced. Specifically, only two V-shaped conveyors were set in the secondary-to-sixth stage formation tanks F2-F6, and only four V-shaped conveyors were set in the seventh stage formation tank F7. At the same time, the formation current in F2 was adjusted to 40 mA / cm. 2 The formation current in F3 and F4 is adjusted to 35mA / cm. 2 In F5, the formation current is adjusted to 32mA / cm. 2 The formation current in F6 and F7 is adjusted to 30mA / cm. 2 .

[0095] Example 4

[0096] The same preparation process as in Example 1 was used to prepare the electroforming foil, except that the number of V-shaped conveyors in the first to fourth eight-stage electroforming tanks was reduced. Specifically, the number of V-shaped conveyors in the first, second, third, and fourth eight-stage electroforming tanks were set to 6, 3, 2, and 1, respectively. At the same time, the electroforming current of F8-1 to F8-4 was adjusted to 30 mA / cm. 2 .

[0097] Example 5

[0098] The same preparation process as in Example 1 was used to prepare the electrolytic foil, except that the number of V-shaped conveyors in the hydration tank and the primary electrolytic formation tank F1 was increased. Specifically, eight V-shaped conveyors were set in the hydration tank and four V-shaped conveyors were set in the primary electrolytic formation tank F1. At the same time, the electrolytic current in F1 was adjusted to 30 mA / cm. 2 .

[0099] Tests revealed that while this embodiment increased the number of V-shaped conveyors, the product quality remained largely unchanged, the reaction time was extended, and power consumption in F1 increased.

[0100] Example 6

[0101] The same preparation process as in Example 1 was used to prepare the chemically formed foil, except that the number of V-shaped conveyors in the secondary-to-seventh stage chemically formed tanks F2-F7 was increased. Specifically, four V-shaped conveyors were set in the secondary-to-sixth stage chemically formed tanks F2-F6, and six V-shaped conveyors were set in the seventh stage chemically formed tank F7.

[0102] Tests revealed that while this embodiment increased the number of V-shaped conveyors, the product quality remained largely unchanged, the response time was extended, and the overall power consumption increased.

[0103] Example 7

[0104] The same preparation process as in Example 1 was used to prepare the chemically formed foil, except that the operating speed was increased, reducing the reaction time of the foil on a single V-shaped conveyor to 90s. At the same time, the number of V-shaped conveyors in the hydration tank and the secondary-seventh stage chemically formed tanks F2-F7 was increased. Specifically, 8 V-shaped conveyors were set in the hydration tank, 4 V-shaped conveyors were set in the primary stage chemically formed tank, 4 V-shaped conveyors were set in each of the secondary-sixth stage chemically formed tanks F2-F6, and 6 V-shaped conveyors were set in the seventh stage chemically formed tank F7.

[0105] Tests revealed that at high speeds, excessive tension on the guide rollers could occur, occasionally causing slight curling at the edges of the material.

[0106] Comparative Example 1

[0107] The same preparation process as in Example 1 was used to prepare the electroforming foil, except that the electroforming tanks F1, F2, F3, F4, F5, F6, F7, F8-1 to F8-4 were powered by a silver roller power supply mode, and the reaction time between the aluminum foil and the tank liquid on each V-shaped conveyor was 240s.

[0108] Comparative Example 2

[0109] The same preparation process as in Example 1 was used to prepare the aluminum foil, and the aluminum foil on each of the formation tanks F1, F2, F3, F4, F5, F6, F7, F8-1 to F8-4 was powered by liquid-fed power supply. The reaction time between the aluminum foil and the tank liquid on each V-shaped conveyor was 150s.

[0110] Comparative Example 3

[0111] The same preparation process as in Example 1 was used to prepare the aluminum foil, except that the power supply mode of the liquid-feed power supply device was changed to a three-stage liquid-feed mode. Specifically, the silver roller supplies power to the first-stage formation tank F1 and the second-stage formation tank F2; the first liquid-feed power supply device supplies power to the third-stage formation tank F3 and the fourth-stage formation tank F4; the second liquid-feed power supply device supplies power to the fifth-stage formation tank F5 and the sixth-stage formation tank F6; and the third liquid-feed power supply device supplies power to the seventh-stage formation tank F7 and the first to fourth eighth-stage formation tanks F8-1 to F8-4. The reaction time between the aluminum foil and the bath liquid on each V-shaped conveyor is 100 seconds. The liquid-feed power supply uses an ammonium adipate solution with a conductivity of 35000.

[0112] Comparative Example 4

[0113] The etched foil is processed using a conventional chemical formation process (refer to existing patent document CN110016703) to obtain the chemically formed foil.

[0114] The electroformed foils obtained in Examples 1 to 7 and Comparative Examples 1 to 4 were subjected to performance tests. The testing equipment included: electroformed foil TV characteristic tester, electroformed foil LCR tester, bending tester, and measuring tank with a capacity of 1000 ml.

[0115] The leakage current, withstand voltage, and withstand voltage rise time were tested using a TV characteristic tester at a temperature of 85℃. The test solution was 1000ml of pure water containing 70g of boric acid, with a resistivity of 7.5±0.3KΩ·cm and a pH of 3.2. The test current was 2.0±0.2mA. During the test, the time it took for the rated diaphragm withstand voltage (Vf) to reach 90% of the voltage (Vr) from the start of power-on was recorded as the rise time. After 3 minutes of testing, the withstand voltage, withstand voltage rise time, and leakage current were read.

[0116] The capacity was tested using an LCR meter. The test solution was 1000ml of pure water containing 80g of ammonium pentaborate, with a resistivity of 30±5Ω·cm, a pH of 7.4, and a test temperature of 30℃.

[0117] Bending data was tested using a bending machine.

[0118] The results are shown in the table below:

[0119] Table 1. Foil performance of examples and comparisons

[0120]

[0121]

[0122] As can be seen from the table above, the present invention is superior to other comparative examples in terms of performance parameters such as withstand voltage, boost time, capacity, leakage current, bending, and total energy consumption. Among them, Example 1 has the best effect, and no flashover or edge curling of liquid-fed power supply occurred during the production process.

[0123] The electrolytic foil obtained in Example 1 was characterized by SEM, and the microstructure of the oxide film formed on its surface is shown in the attached figure. Figure 5 As shown, under the conditions of high vehicle speed and low energy consumption in Example 1, the alumina film generated by its formation has a regular, dense, and stable structure, which brings it better voltage resistance, lower leakage current, and shorter voltage boost time. This reduces its cost while improving its overall performance, thus better meeting market demands.

[0124] The above embodiments are merely preferred embodiments of the present invention, and the scope of protection of the present invention is not limited to the above embodiments. All technical solutions falling within the scope of the present invention's concept are within the scope of protection of the present invention. It should be noted that for those skilled in the art, improvements and modifications made without departing from the principles of the present invention should also be considered within the scope of protection of the present invention.

Claims

1. A multi-stage formation method for preparing anode foil for aluminum electrolytic capacitors, characterized in that, It includes: The aluminum etched foil is subjected to the following sequential processes via a continuously conveying V-shaped conveyor: hydration treatment, primary formation treatment in the first treatment solution, secondary formation treatment in the second treatment solution, tertiary formation treatment in the third treatment solution, quaternary formation treatment in the fourth treatment solution, quinary formation treatment in the fifth treatment solution, sixth formation treatment in the sixth treatment solution, seventh formation treatment in the seventh treatment solution, octet formation treatment in the first octet solution, octet formation treatment in the second octet solution, and octet formation treatment in the third octet solution. The third and eighth-stage formation processes and the fourth and eighth-stage formation processes performed in the fourth and eighth-stage processing solution; wherein the formation voltages of the first, second, third, fourth, fifth, sixth, seventh, first and eighth-stage formation processes, second and eighth-stage formation processes, third and eighth-stage formation processes are 100V, 180V, 260V, 340V, 410V, 480V, 510V, 530V, 530V, 530V, and 530V, respectively, and the formation currents are 30-50mA / cm. 2 30-40mA / cm 2 30-45mA / cm 2 30-35mA / cm 2 26-32mA / cm 2 25-30mA / cm 2 25-30mA / cm 2 25-30mA / cm 2 25-30mA / cm 2 25-30mA / cm 2 25-30mA / cm 2 The V-shaped conveyor consists of three guide rollers arranged in a V-shape, specifically including: two drive rollers of equal height at the top and a bottom roller located in the middle below the two drive rollers. The contact time between the foil material on each V-shaped conveyor and each treatment liquid is 100-120 seconds. The hydration treatment, primary treatment, secondary formation treatment, tertiary formation treatment, quaternary formation treatment, quinary formation treatment, sixth formation treatment, seventh formation treatment, first octave formation treatment, second octave formation treatment, third octave formation treatment, and fourth octave formation treatment are all described. The number of V-shaped conveyors used are 6-7, 2-3, 2-3, 2-3, 2-3, 2-3, 2-3, 4-5, 6-7, 3-4, 2-3, and 1-2 respectively; and the first-stage formation process adopts a silver roller power supply method, while the second-stage, third-stage, fourth-stage, fifth-stage, sixth-stage, seventh-stage, first eighth-stage, second eighth-stage, third eighth-stage, and fourth eighth-stage formation processes all adopt a liquid-fed power supply method.

2. The multi-stage formation method according to claim 1, characterized in that, The multi-stage formation method further includes: a first phosphoric acid treatment following the first eight-stage formation process, a second phosphoric acid treatment following the second eight-stage formation process, and a post-processing following the fourth eight-stage formation process, wherein the number of V-shaped conveyors used in the first phosphoric acid treatment, the second phosphoric acid treatment, and the post-processing are 1, 3, and 2, respectively.

3. The multi-stage formation method according to claim 1, characterized in that, The first treatment solution comprises: a mixed aqueous solution of ammonium adipate (3-5 g / L), boric acid (8-10 g / L), ammonium azelate (3-5 g / L), sodium hypophosphite (1-2 g / L), and citric acid (4-5 g / L); the second treatment solution comprises: a mixed aqueous solution of ammonium adipate (2-4 g / L), boric acid (8-10 g / L), ammonium azelate (2.5-4 g / L), sodium hypophosphite (1-2 g / L), and citric acid (4-5 g / L); the third treatment solution comprises: a mixed aqueous solution of boric acid (20-40 g / L), citric acid (2-6 g / L), and ammonium azelate (5-7 g / L); the fourth treatment solution comprises: a mixed aqueous solution of boric acid (50-60 g / L), citric acid (2 g / L), and sodium azelate (2 g / L). The fifth treatment solution comprises: a mixed aqueous solution of citric acid at a concentration of 50-60 g / L and ammonium azelate at a concentration of 4-6 g / L; the sixth treatment solution comprises: a mixed aqueous solution of boric acid at a concentration of 50-60 g / L and ammonium pentaborate at a concentration of 3-5 g / L; the seventh treatment solution comprises: a mixed aqueous solution of boric acid at a concentration of 50-60 g / L and ammonium pentaborate at a concentration of 3-5 g / L; the first, second, third, and fourth eighth-stage treatment solutions all comprise: a mixed aqueous solution of boric acid at a concentration of 50-60 g / L and ammonium pentaborate at a concentration of 3-5 g / L.

4. The multi-stage formation method according to claim 1, characterized in that, Specifically, it includes: conveying foil material through the V-shaped conveyor, and performing the following sequentially: (1) Boil the aluminum etched foil in pure water at 92~98℃ to obtain the hydration-treated foil; (2) The hydrated foil is subjected to a first-stage formation treatment in a first-stage treatment solution to obtain a first-stage treated foil; the first-stage treatment solution comprises: a mixed aqueous solution of ammonium adipate (3-5 g / L), boric acid (8-10 g / L), ammonium azelate (3-5 g / L), sodium hypophosphite (1-2 g / L), and citric acid (4-5 g / L). During the formation treatment, the temperature of the first-stage treatment solution is controlled at 80-90°C, the formation voltage is 100 V, and the formation current is 30-50 mA / cm. 2 ; (3) The primary-treated foil is subjected to a secondary formation process in a second-treatment solution to obtain a secondary-treated foil; the second-treatment solution comprises: a mixed aqueous solution of ammonium adipate (2-4 g / L), boric acid (8-10 g / L), ammonium azelaate (2.5-4 g / L), sodium hypophosphite (1-2 g / L), and citric acid (4-5 g / L). During the formation process, the temperature of the second-treatment solution is controlled at 85±5℃, the formation voltage is 180V, and the formation current is 30-40mA / cm. 2 ; (4) The secondary-treated foil is sprayed and washed with water, and then subjected to a tertiary formation process in a third treatment solution to obtain a tertiary-treated foil; the third treatment solution includes a mixed aqueous solution of boric acid with a concentration of 20-40 g / L, citric acid with a concentration of 2-6 g / L, and ammonium azelate with a concentration of 5-7 g / L. During the formation process, the temperature of the third treatment solution is controlled at 85±5℃, the formation voltage is 260V, and the formation current is 30-45mA / cm. 2 ; (5) The three-stage treated foil is immersed and washed with water, and then subjected to a four-stage formation treatment in a fourth treatment solution to obtain a four-stage treated foil; the fourth treatment solution includes a mixed aqueous solution of boric acid (50-60 g / L), citric acid (2-6 g / L), and ammonium azelate (4-6 g / L). During the formation treatment, the temperature of the fourth treatment solution is controlled at 85±5℃, the formation voltage is 340V, and the formation current is 30-35mA / cm. 2 ; (6) The fourth-stage treated foil is sprayed and washed with water, and then subjected to a fifth-stage formation process in a fifth treatment solution to obtain a fifth-stage treated foil. The fifth treatment solution comprises a mixed aqueous solution of boric acid (50-60 g / L), citric acid (2-6 g / L), and ammonium azelate (4-6 g / L). During the formation process, the temperature of the fourth treatment solution is controlled at 85±5℃, the formation voltage is 410V, and the formation current is 26-32mA / cm. 2 ; (7) The fifth-stage treated foil is sprayed and washed with water, and then subjected to a sixth-stage formation process in a sixth-stage treatment solution to obtain a sixth-stage treated foil. The sixth-stage treatment solution includes a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation process, the temperature of the fifth-stage treatment solution is controlled at 85±5℃, the formation voltage is 480V, and the formation current is 25-30mA / cm. 2 ; (8) The sixth-stage treated foil is sprayed and washed with water, and then subjected to a seventh-stage formation process in a seventh-stage treatment solution to obtain a seventh-stage treated foil. The seventh-stage treatment solution includes a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation process, the temperature of the fifth-stage treatment solution is controlled at 85±5℃, the formation voltage is 510V, and the formation current is 25-30mA / cm. 2 ; (9) The seventh-stage treated foil is immersed and washed with water, and then subjected to a first-eighth-stage formation treatment in a first-eighth-stage treatment solution to obtain a first-eighth-stage treated foil. The first-eighth-stage treatment solution includes a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation treatment, the temperature of the first-eighth-stage treatment solution is controlled at 85±5℃, the formation voltage is 530V, and the formation current is 25-30mA / cm. 2 ; (10) The first eighth-level treated foil is washed with water and then subjected to phosphoric acid treatment at 55±5℃ in the first phosphoric acid solution. The treated foil is washed with water and then calcined at 520-550℃ for 2 minutes to obtain the first heat-treated foil. The mass percentage concentration of the first phosphoric acid solution is 5%. (11) The first heat-treated foil is subjected to a second-eighth-stage formation process in a second-eighth-stage processing solution to obtain a second-eighth-stage treated foil. The second-eighth-stage processing solution comprises a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation process, the temperature of the second-eighth-stage processing solution is controlled at 85±5℃, the formation voltage is 530 V, and the formation current is 25-30 mA / cm. 2 ; (12) After washing the second eighth-stage treated foil with water, immerse it in the second phosphoric acid solution for 150-180s, and then wash it with water to obtain a water-washed foil. The mass percentage concentration of the second phosphoric acid solution is 10%. (13) The washed foil is subjected to a third-eighth-stage formation treatment in a third-eighth-stage treatment solution to obtain a third-eighth-stage treated foil. The third-eighth-stage treatment solution comprises a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation treatment, the temperature of the third-eighth-stage treatment solution is controlled at 85±5℃, the formation voltage is 530V, and the formation current is 25-30mA / cm. 2 ; (14) The third grade eight-stage treated foil is washed with water and then calcined at 420-500℃ for 2 minutes to obtain the second heat-treated foil; (15) The second heat-treated foil is subjected to a fourth-eighth-stage formation process in a fourth-eighth-stage processing solution to obtain a fourth-eighth-stage treated foil. The fourth-eighth-stage processing solution comprises a mixed aqueous solution of boric acid with a concentration of 50-60 g / L and ammonium pentaborate with a concentration of 3-5 g / L. During the formation process, the temperature of the fourth-eighth-stage processing solution is controlled at 85±5℃, the formation voltage is 530 V, and the formation current is 25-30 mA / cm. 2 ; (16) The fourth and eighth grade processed foil is washed with water and then immersed in a 6 g / L ammonium dihydrogen phosphate solution, followed by washing and drying to obtain the chemically processed foil.

5. The multi-stage formation method according to claim 4, characterized in that, The secondary, tertiary, quaternary, quinary, sixth, seventh, first octet, second octet, third octet, and fourth octet formation processes are all achieved by liquid-feed power supply devices. The primary formation process is achieved by silver roller power supply, which is powered by a silver conductive roller that is connected to the V-shaped conveyor and connected to the power source. The conductive liquid used in the liquid-feed power supply device is an ammonium adipate solution with a conductivity of 35,000.

6. A formation system for implementing the multi-stage formation method according to any one of claims 1-5, comprising: The hydration treatment, primary formation treatment, secondary formation treatment, tertiary formation treatment, quaternary formation treatment, quinary formation treatment, sixth formation treatment, seventh formation treatment, first octave formation treatment, second octave formation treatment, third octave formation treatment, and fourth octave formation treatment are carried out in separate hydration tanks, primary formation tanks, secondary formation tanks, tertiary formation treatments, quaternary formation treatments, quinary formation treatments, sixth formation treatments, seventh formation treatments, first octave formation treatment, second octave formation treatment, third octave formation treatment, and fourth octave formation treatment. Each formation tank is equipped with several V-shaped conveyors. Each V-shaped conveyor consists of three guide rollers arranged in a V-shape, specifically including two drive rollers of equal height at the top and a bottom roller located below the two drive rollers in the middle. The foil material on the V-shaped conveyor contacts the tank liquid. The time is 100-120s; the number of V-shaped conveyors in the hydration tank, primary formation tank, secondary formation tank, tertiary formation tank, quaternary formation tank, quinary formation tank, sixth formation tank, seventh formation tank, first octave formation tank, second octave formation tank, third octave formation tank, and fourth octave formation tank are 6-7, 2-3, 2-3, 2-3, 2-3, 2-3, 4-5, 6-7, 3-4, 2-3, and 1-2, respectively; and the primary formation process uses a silver roller power supply method, while the secondary, tertiary, quaternary, quinary, sixth, seventh, first octave formation tank, second octave formation tank, third octave formation tank, and fourth octave formation tank all use a liquid-fed power supply method.

7. The formation system according to claim 6, characterized in that, It also includes: a first phosphoric acid tank located between the first eight-stage formation tank and the second eight-stage formation tank; a second phosphoric acid tank located between the second eight-stage formation tank and the third eight-stage formation tank; and a post-treatment tank located after the fourth eight-stage formation tank; a plurality of V-shaped conveyors are provided in the hydration tank, the first phosphoric acid tank, the second phosphoric acid tank, and the post-treatment tank; the number of V-shaped conveyors provided in the first phosphoric acid tank, the second phosphoric acid tank, and the post-treatment tank are 1, 3, and 2, respectively.

8. The formation system according to claim 6, characterized in that, It also includes: a first liquid-feed power supply device for supplying power to the secondary formation tank and the tertiary formation tank; a second liquid-feed power supply device for supplying power to the quaternary formation tank and the quinary formation tank; a third liquid-feed power supply device for supplying power to the sixth formation tank and the seventh formation tank; and a fourth liquid-feed power supply device for supplying power to the first octave formation tank, the second octave formation tank, the third octave formation tank, and the fourth octave formation tank.

9. The formation system according to claim 6, characterized in that, It also includes a silver conductive roller located in front of the hydration tank and connected to the V-shaped conveyor inside the hydration tank, the silver conductive roller being connected to a power source.

10. A formed foil obtained by any one of the multi-stage formation methods according to claims 1-5 or by any one of the multi-stage formation systems according to claims 7-9.

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