A clamp with adjustable tension and a test device for corrosion foil and a preparation method thereof

Abstract

This invention relates to the field of laboratory preparation technology for corrosion foil, and more specifically, to an adjustable tension clamp and a method for preparing a testing device for corrosion foil. The adjustable tension clamp includes a suspension frame, a slide rail, a support frame, a fixed clamping plate structure for clamping one end of an aluminum foil, and a movable clamping plate structure for clamping the other end of the aluminum foil. The slide rail connects the suspension frame and the support frame. The fixed clamping plate structure is fixedly mounted on the suspension frame. The suspension frame has a through hole for the aluminum foil to pass through. The movable clamping plate structure is slidably mounted on the slide rail. The movable clamping plate structure is also connected to a driving structure for driving the movable clamping plate structure to slide. This invention, by adjusting the distance between the movable clamping plate structure and the fixed clamping plate structure, can thereby adjust the tension on the aluminum foil. Using this clamp in the laboratory preparation of corrosion foil fills the gap in current laboratory simulations regarding the lack of research on the effects of tension adjustment on the performance of corrosion foil.

Description

Technical Field

[0001] The invention relates to the technical field of laboratory preparation of corrosion foil, and more particularly to a clamp with adjustable tension and a preparation method of a test device for corrosion foil. Background Art

[0002] Anodic foil is the main raw material of aluminum electrolytic capacitors, and its corrosion specific capacitance is the key parameter of aluminum electrolytic capacitor capacitance. Therefore, the manufacturing technology of electrode foil largely determines the technical level of aluminum electrolytic capacitors. In order to adjust and optimize the production process of corrosion foil, a small sample electrolytic corrosion tank is usually customized in the laboratory to simulate the production process and parameters to guide production, such as current, electric field, tank liquid concentration, production process and cycle rate.

[0003] However, in the actual continuous production process of corrosion electrode foil, due to the use of a large number of conveyor rollers, the transmission between the rollers causes the foil to be stretched to varying degrees. The stretching of the foil will inevitably affect the microscopic cubic texture of the aluminum foil, the uniformity of the surface oxide film, and the thickness of the foil, thereby having a certain impact on the performance of the corrosion foil.

[0004] The production process and parameters simulated by the existing laboratory sample electrolytic corrosion tank mainly include current, electric field, tank solution concentration, production process and cycle rate, etc. There is no information on the preparation method of laboratory corrosion samples under tension conditions, the effect of tension on the corrosion process, and the corrosion products under adjustable tension conditions, etc. For example, the existing fixture of the small sample electrolytic corrosion foil only provides support for the aluminum foil, and cannot provide tension or adjustable tension.

[0005] In the laboratory, due to the lack of research experience on the effect of tension adjustment on the performance of corrosion foil, the laboratory simulation results often differ from the production verification results, which greatly reduces the feasibility of laboratory results in production and lacks substantial guidance. The production guidance value of laboratory research and development results is greatly reduced. Therefore, developing a laboratory preparation device for corrosion foil under adjustable tension conditions and studying the effect of tension on the performance of corrosion foil is conducive to improving the consistency between laboratory simulation results and production line performance, which has important guiding significance for the production of high-performance anodized foil and the large-scale production of high-specific capacitance aluminum electrolytic capacitors.

[0006] For example, the prior art discloses a tension-adjusting jumping roller device for a corrosion foil production line, comprising an active roller, a jumping roller, a bracket, an adjusting shaft, a counterweight box, a collecting vessel, a screw conveyor, an output structure and a tension sensor, wherein the active rollers are fixed on the same horizontal line, the jumping roller is centrally arranged below the two active rollers, the corrosion foil passes around the active roller and the jumping roller to form a triangle shape, the bracket is arranged on one side of the jumping roller, the adjusting shaft is mounted on the bracket, one end of the adjusting shaft is connected to the top of the jumping roller, and the other end is provided with a counterweight box, spherical counterweight particles are contained in the counterweight box, counterweight particles are arranged at the bottom, and an output structure for the counterweight particles is arranged at the bottom, the collecting vessel is placed below the counterweight box, and the screw conveyor is placed above the top of the counterweight box; the tension sensor is placed on the edge of the aluminum foil, and the tension-adjusting jumping roller device can implement tension monitoring and adjustment to improve product quality, but the tension-adjusting jumping roller device is only suitable for applications in actual production, and is not suitable for laboratory preparation and testing of corrosion foil. Summary of the invention

[0007] The present invention overcomes the problem of lack of research experience on the effect of tension adjustment on the performance of corrosion foil in the laboratory simulation process described in the prior art, and provides a fixture with simple structure and adjustable tension and a preparation method of a test device for corrosion foil.

[0008] In order to solve the above technical problems, the technical solution adopted by the present invention is: a clamp with adjustable tension, including a hanging frame, a sliding rail, a supporting frame, a fixed clamping plate structure for clamping one end of the aluminum foil and a movable clamping plate structure for clamping the other end of the aluminum foil; the sliding rail is connected between the hanging frame and the supporting frame; the fixed clamping plate structure is fixed on the hanging frame; the hanging frame is provided with a through hole for the aluminum foil to pass through; the movable clamping plate structure is slidably arranged on the sliding rail; the movable clamping plate structure is also connected to a driving structure for driving the movable clamping plate structure to slide.

[0009] The fixed clamping plate structure of the present invention is fixedly arranged on a hanging frame, and the movable clamping plate structure can slide on a slide rail. The movable clamping plate structure is driven to move by a driving structure. When in use, one end of the aluminum foil is passed through a through hole on the hanging frame and fixed on the fixed clamping plate structure, and the other end of the aluminum foil is fixed on the movable clamping plate structure. By adjusting the distance between the movable clamping plate structure and the fixed clamping plate structure, the tension applied to the aluminum foil can be adjusted. The clamp is used in laboratory preparation of corrosion foil, which can fill the gap in the research on the performance of corrosion foil due to the lack of tension adjustment in the current laboratory simulation process, and has positive guiding significance for the production of formed foil and the large-scale production of high-specific-capacity aluminum electrolytic capacitors in actual production.

[0010] Preferably, the fixed clamping plate structure includes a first clamping plate, a second clamping plate and a first fixing assembly for fixing the aluminum foil between the first clamping plate and the second clamping plate; the first clamping plate and the second clamping plate are arranged on a hanging frame; the first fixing assembly is arranged on the first clamping plate and / or the second clamping plate.

[0011] Preferably, the movable clamping plate structure comprises a clamping member slidably connected to the slide rail and a second fixing component for fixing the aluminum foil on the clamping member; the second fixing component is connected to the clamping member.

[0012] Preferably, the clamping member is provided with a protrusion; the slide rail is provided with a slide groove; the slide groove is slidably connected to the protrusion.

[0013] Preferably, the driving structure comprises a screw connected to the clamping member; and the support frame is provided with a third threaded hole that matches the thread of the screw.

[0014] Preferably, the screw rod is provided with scales; the spacing between the scales is 1 to 4 mm.

[0015] A method for preparing a test device for a corrosion foil, using the above-mentioned fixture to adjust the tension of the corrosion foil, specifically comprises the following steps:

[0016] S1: Fixing foil: Cut the high-pressure light foil into foils of required size, and then fix one end of the foil on the fixed clamping plate structure and the other end on the movable clamping plate structure;

[0017] S2: Adjust the foil tension: The driving structure drives the movable clamping plate structure to move on the slide rail, thereby changing the distance between the fixed clamping plate structure and the movable clamping plate structure. The tension at both ends of the foil can be calculated according to Hooke's law.

[0018] S3: Corrosion treatment: The foil with tension adjusted in step S2 is subjected to corrosion treatment under laboratory conditions to obtain a corroded foil.

[0019] Preferably, the thickness of the high pressure light foil in step S1 is 115-145 μm, the purity is greater than 99.99%, and the cubic texture is greater than 95%.

[0020] Preferably, in the steps, the moving distance of the movable clamping plate structure in step S2 is 0-50 mm, which corresponds to the tension of 0-250 kN on both ends of the foil.

[0021] Preferably, step S3 includes the following specific steps:

[0022] S31: The foil with tension adjusted in step S2 is immersed in a sodium hydroxide solution with a temperature of 310-330K and a concentration of 0.225-0.275 mol / L for 2.5-3.5 min, and then immersed in a mixed acid of a hydrochloric acid solution and a sulfuric acid solution with a volume ratio of (0.5-5):1 at a temperature of 320-345K for 1.5-2.5 min to remove the surface oxide film and oil film, wherein the concentration of the hydrochloric acid solution is 0.8-1.2 mol / L, and the concentration of the sulfuric acid solution is 3.0-4.0 mol / L, and then immersed in deionized water for standby use;

[0023] S32: The foil obtained in step S31 is used as an anode, and a fixture is fixed in a corrosion tank and a porous foil is obtained by direct current corrosion in a mixed acid of a hydrochloric acid solution and a sulfuric acid solution at a temperature of 335-355K and a volume ratio of (0.5-5):1, wherein the concentration of the hydrochloric acid solution is 0.8-1.2 mol / L, the concentration of the sulfuric acid solution is 3.0-4.0 mol / L, and the average corrosion current density is 0.25-0.35 A / cm 2 , corrosion time is 140~160s:

[0024] S33: Etching and expanding the hole: The perforated foil obtained in step S32 is subjected to secondary hole expansion etching in a 0.45-0.55 mol / L nitric acid solution at 330-350 K, with a corrosion current density of 0.15-0.20 A / cm 2 , the etching time is 250-300s. After hole expansion, the foil is immersed in deionized water for 35-40min and then dried;

[0025] S34: treating the corroded foil obtained in step S33 in a nitric acid solution with a weight percentage of 4.5-5.5wt% for 2.5-3.5min at a temperature of 60-70°C, taking out the corroded foil, and drying it for later use.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] 1) The tension-adjustable clamp of the present invention can adjust the displacement of the movable clamping structure on the slide rail, thereby adjusting the tension of the foil. The overall structure is simple to set and easy to operate, and is suitable for adjusting the tension of the foil under laboratory conditions;

[0028] 2) The present invention uses a tension-adjustable clamp in the preparation of a test device for corrosion foil, which can fill the gap in the current research on corrosion foil performance due to the lack of tension adjustment in the laboratory simulation process, and can greatly improve the consistency between laboratory simulation results and production line performance, thereby improving the production guidance significance of laboratory research results. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1It is a structural schematic diagram of the tension-adjustable clamp of the present invention;

[0030] Figure 2 It is a structural schematic diagram of another angle of the tension-adjustable clamp of the present invention;

[0031] Figure 3 It is a schematic diagram of the matching structure of the movable splint structure and the slide rail in the present invention;

[0032] Figure 4 It is a schematic diagram of the bottom structure of the movable splint structure of the present invention;

[0033] Figure 5 It is a schematic diagram of the structure of the foil of the present invention being fixed on a clamp with adjustable tension;

[0034] Figure 6 The present invention is a flow chart of a method for preparing a test device for etching foil.

[0035] In the accompanying drawings: 1-suspension frame; 2-slide rail; 21-slide groove; 3-support frame; 31-third threaded hole; 4-fixed clamping plate structure; 41-first clamping member; 42-second clamping member; 43-first fixing assembly; 431-first threaded hole; 432-first nut; 5-movable clamping plate structure; 51-clamping member; 511-third clamping member; 512-fourth clamping member; 513-bottom plate; 52-second fixing structure; 521-second threaded hole; 522-second nut; 53-protrusion; 6-driving structure; 61-screw; 10-aluminum foil. DETAILED DESCRIPTION

[0036] The drawings are only for illustrative purposes and cannot be construed as limiting the present invention. To better illustrate the present embodiment, some parts of the drawings may be omitted, enlarged, or reduced, and do not represent the size of the actual product. For those skilled in the art, it is understandable that some well-known structures and their descriptions may be omitted in the drawings. The positional relationships described in the drawings are only for illustrative purposes and cannot be construed as limiting the present invention.

[0037] The same or similar numbers in the drawings of the embodiments of the present invention correspond to the same or similar parts; in the description of the present invention, it should be understood that if the terms "upper", "lower", "left", "right", "long", "short" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, they are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes and cannot be understood as limitations on this patent. For ordinary technicians in this field, the specific meanings of the above terms can be understood according to specific circumstances.

[0038] The technical solution of the present invention is further described in detail below through specific embodiments and in conjunction with the accompanying drawings:

[0039] Example 1

[0040] like Figure 1-Figure 6 The invention shows an embodiment 1 of a clamp with adjustable tension and a method for preparing a test device for corrosion foil, wherein the clamp with adjustable tension comprises a suspension frame 1, a slide rail 2, a support frame 3, a fixed clamping plate structure 4, a movable clamping plate structure 5 and a driving structure 6, wherein the suspension frame 1 is a plate-like structure, the fixed clamping plate structure 4 is arranged on the top of the suspension frame 1, one end of the slide rail 2 is connected to the bottom of the suspension frame 1, and the other end is connected to the support frame 3, wherein the movable clamping plate structure 5 is slidably arranged on the slide rail 2, wherein the driving structure 6 can drive the movable clamping plate structure 5 to slide on the slide rail 2, during use, the fixed clamping plate structure 4 is used to fix one end of the aluminum foil, and the movable clamping plate structure 5 is used to fix the other end of the aluminum foil, and the tension applied to the aluminum foil can be adjusted by adjusting the spacing between the movable clamping plate structure 5 and the fixed clamping plate structure 4.

[0041] As a preferred technical solution, in order to improve the stability of the movable clamping plate structure 5 moving on the slide rail 2, two slide rails 2 are provided, which are respectively located at the two ends of the bottom of the suspension frame 1, and the movable clamping plate structure 5 can move on the two slide rails 2.

[0042] Specifically, the fixed clamping plate structure 4 includes a first clamping member 41, a second clamping member 42 and a first fixing assembly 43, wherein the first clamping member 41 and the second clamping member 42 are arranged on the top of the hanging frame 1, the first clamping member 41 and the second clamping member 42 are arranged parallel to each other, and there is a certain interval between the first clamping member 41 and the second clamping member 42, wherein the hanging frame 1 is provided with a through hole for the aluminum foil 10 to pass through, due to viewing angle reasons, the through hole is not shown in the accompanying drawings, specifically, the through hole is located on the hanging frame 1 between the first clamping member 41 and the second clamping member 42, and the through hole allows the aluminum foil 10 to extend from the hanging frame 1 to between the first clamping member 41 and the second clamping member 42.

[0043] The first fixing component 43 can fix one end of the aluminum foil between the first clamping member 41 and the second clamping member 42. Specifically, the first fixing component 43 includes a first threaded hole 431 and a first nut 432, wherein the first threaded hole 431 is arranged on the first clamping plate 41 or the second clamping plate 42. In this embodiment, the first threaded hole 431 is arranged on the first clamping plate 41, and the first nut 432 is screwed on the first threaded hole 431. By tightening the first nut 432 to fix the aluminum foil between the first nut 432 and the second clamping member 42, one end of the aluminum foil can be firmly fixed between the first clamping member 41 and the second clamping member 42.

[0044] Specifically, the movable clamping plate structure 5 includes a clamping member 51 and a second fixed component 52, and the clamping member 51 can be slidably connected on the slide rail 2. In this embodiment, the clamping member 51 is movably sleeved on the slide rail 2, and the bottom of the clamping member 51 is provided with a through hole for the two slide rails 2 to pass through. Specifically, the clamping member 51 includes a third clamping plate 511, a fourth clamping plate 512 and a bottom plate 513, wherein the third clamping plate 511 and the fourth clamping plate 512 are fixed on the bottom plate 513, and the lengths of the third clamping plate 511 and the fourth clamping plate 512 are both greater than the length of the bottom plate 513. Therefore, when the third clamping member 511 and the fourth clamping member 512 are arranged on the bottom plate 513, a through hole for the two slide rails 2 to pass through can be formed on the clamping member 51, so that the clamping member 51 can be slidably sleeved on the slide rail 2.

[0045] As a preferred technical solution, in this embodiment, a protrusion 53 is provided on the clamping member 51. Specifically, the protrusion 53 can be arranged on the third clamping plate 511 and / or the fourth clamping plate 512. In this embodiment, the protrusion 53 is arranged on the third clamping member 511, wherein a sliding groove 21 is provided on the slide rail 2, and the sliding groove 21 is slidably connected with the protrusion 53. When the clamping member 51 moves on the slide rail 2, the protrusion 53 can slide in the sliding groove 21, wherein the setting of the protrusion 53 and the sliding groove 21 can improve the stability of the clamping member 51 sliding on the slide rail 2.

[0046] The second fixing component 52 can fix the other end of the aluminum foil on the clamping member 51. Specifically, the second fixing component 52 includes a second threaded hole 521 and a second nut 522, wherein the second threaded hole 521 is arranged on the third clamping plate 511 and / or the fourth clamping plate 512. In this embodiment, the second threaded hole 521 is arranged on the third clamping plate 51. By tightening the second nut 522 to fix the aluminum foil between the second nut 522 and the fourth clamping member 512, one end of the aluminum foil can be firmly fixed on the clamping member 51.

[0047] The driving structure 6 is used to drive the movable clamping plate structure 5 to slide up and down on the slide rail 1. Specifically, the driving structure 6 includes a screw 61, wherein a third threaded hole 31 is provided on the support frame 3, wherein the screw 61 is screwed on the third threaded hole 31, and the screw 61 can drive the clamping member 51 to move on the slide rail 2 through the cooperation of the screw 61 and the third threaded hole 31.

[0048] The screw rod 61 is provided with a scale, wherein the scale interval is 1 to 4 mm, and in this embodiment the scale interval is 1 mm. The scale range on the screw rod 61 is 0 to 50 mm, wherein the scale position 0 is when the aluminum foil has no tension, and the scale position 50 is the maximum traction distance.

[0049] The specific working principle of the above-mentioned adjustable tension clamp is:

[0050] When in use, one end of the aluminum foil 10 is passed through the through hole of the suspension frame 1 and fixed between the first clamping plate 41 and the second clamping plate 42 through the first fixing component 43, and the other end of the aluminum foil 10 is fixed on the clamping member 51, and the clamping member 51 is driven to slide on the slide rail 2 by the screw 61. By adjusting the displacement of the clamping member 51 on the slide rail 2, the tension exerted on the aluminum foil 10 can be calculated according to Hooke's law. The entire structure is simple to set up and easy to use. The use of the tension-adjustable clamp in the laboratory preparation of corrosion foil can fill the gap in the current laboratory simulation process for the study of corrosion foil performance due to the lack of tension adjustment, and can greatly improve the consistency between the laboratory simulation results and the production line performance, thereby improving the production guidance significance of the laboratory research results.

[0051] A method for preparing a test device for a corrosion foil, using the above-mentioned tension-adjustable fixture to adjust the tension of the corrosion foil, specifically comprises the following steps:

[0052] S1: Fixing the foil: Cut the high-pressure optical foil with a thickness of 130 μm, a purity greater than 99.99%, and a cubic texture greater than 95% into foils of a certain size of 9 cm×15 cm, fix one end of the foil between the first clamping plate 41 and the second clamp 42 through the first nut 432, and fix the other end of the foil on the clamp 51 through the second nut 522.

[0053] S2: Adjusting the tension of the foil: The movable clamping plate structure 5 is driven to move on the slide rail 2 by the driving structure 6. Specifically, the screw 61 is rotated to drive the clamping member 51 to move on the slide rail 2, thereby changing the distance between the fixed clamping plate structure 4 and the movable clamping plate structure 5. The tension at both ends of the foil can be calculated according to Hooke's law. In this embodiment, the moving distance of the movable clamping plate structure 5 of 0 to 50 mm corresponds to the tension at both ends of the foil of 0 to 250 kN, that is, the moving distance of the movable clamping plate structure 5 is 0, that is, the movable clamping plate structure 5 does not move, and the tension at both ends of the foil is 0. The foil is in a natural state and is not subjected to force. When the movable clamping plate structure 5 moves 50 mm away from the fixed clamping plate structure 4, the tension at both ends of the foil is 250 kN. When the moving distance of the movable clamping plate structure 5 away from the fixed clamping plate structure 4 is between 0 and 50 mm, the tension at both ends of the foil can be calculated according to Hooke's law.

[0054] In this embodiment, the tension is set to 0 kN, that is, no tension is provided at both ends of the aluminum foil.

[0055] S3: Corrosion treatment: The foil with tension adjusted in the above step S2 is corroded under laboratory conditions to obtain a corroded foil. The specific operation steps are as follows:

[0056] S31: the foil with tension adjusted in step S2 is immersed in a sodium hydroxide solution with a temperature of 310K and a concentration of 0.225mol / L for 2.5min, and then immersed in a mixed acid of a hydrochloric acid solution and a sulfuric acid solution with a temperature of 320K and a volume ratio of 0.5:1 for 1.5min to remove the surface oxide film and oil film, wherein the concentration of the hydrochloric acid solution is 0.8mol / L and the concentration of the sulfuric acid solution is 3.0mol / L, and then immersed in deionized water for standby use;

[0057] S32: The foil obtained in step S31 is used as an anode, and the fixture is fixed in the corrosion tank and DC corrosion is carried out in a mixed acid of hydrochloric acid solution and sulfuric acid solution at a temperature of 335K and a volume ratio of 0.5:1 to obtain a perforated foil, wherein the concentration of the hydrochloric acid solution is 0.8 mol / L, the concentration of the sulfuric acid solution is 3.0 mol / L, and the average corrosion current density is 0.25 A / cm 2 , the corrosion time is 140s:

[0058] S33: Etching and expanding the hole: The perforated foil obtained in step S32 is subjected to secondary hole expansion etching in a 0.45 mol / L nitric acid solution at 330 K, with a corrosion current density of 0.15 A / cm 2 , the etching time was 250s. After hole expansion, the foil was immersed in deionized water for 35min and then dried;

[0059] S34: treating the corroded foil obtained in step S33 in a nitric acid solution with a weight percentage of 4.5 wt % for 2.5 min at a temperature of 60° C., taking out the corroded foil, and drying it for later use.

[0060] Example 2

[0061] This embodiment is a second embodiment of a method for preparing a test device for etching foil using a clamp with adjustable tension and the same. The difference between this embodiment and the first embodiment is that the method for preparing a test device for etching foil in this embodiment specifically includes the following steps:

[0062] S1: Fixing the foil: Cut the high-pressure optical foil with a thickness of 130 μm, a purity greater than 99.99%, and a cubic texture greater than 95% into foils of a certain size of 9 cm×15 cm, fix one end of the foil between the first clamping plate 41 and the second clamp 42 through the first nut 432, and fix the other end of the foil on the clamp 51 through the second nut 522.

[0063] S2: Adjusting the tension of the foil: The movable clamping plate structure 5 is driven to move on the slide rail 2 by the driving structure 6. Specifically, the screw 61 is rotated to drive the clamping member 51 to move on the slide rail 2, thereby changing the distance between the fixed clamping plate structure 4 and the movable clamping plate structure 5. The tension at both ends of the foil can be calculated according to Hooke's law. In this embodiment, the moving distance of the movable clamping plate structure 5 of 0 to 50 mm corresponds to the tension of 0 to 250 kN at both ends of the foil, that is, the moving distance of the movable clamping plate structure 5 is 0, that is, the movable clamping plate structure 5 does not move. At this time, the tension at both ends of the foil is 0, and the foil is in a natural state without being subjected to force; and when the movable clamping plate structure 5 moves 50 mm away from the fixed clamping plate structure 4, the tension at both ends of the foil is 250 kN. When the moving distance of the movable clamping plate structure 5 away from the fixed clamping plate structure 4 is between 0 and 50 mm, the tension at both ends of the foil can be calculated according to Hooke's law.

[0064] In this embodiment, the tension is set to 0 kN, that is, no tension is provided at both ends of the aluminum foil.

[0065] S3: Corrosion treatment: The foil with tension adjusted in the above step S2 is corroded under laboratory conditions to obtain a corroded foil. The specific operation steps are as follows:

[0066] S31: the foil with tension adjusted in step S2 is immersed in a sodium hydroxide solution with a temperature of 330K and a concentration of 0.275mol / L for 3.5min, and then immersed in a mixed acid of a hydrochloric acid solution and a sulfuric acid solution with a volume ratio of 5:1 at a temperature of 345K for 2.5min to remove the surface oxide film and oil film, wherein the concentration of the hydrochloric acid solution is 1.2mol / L and the concentration of the sulfuric acid solution is 4.0mol / L, and then immersed in deionized water for standby use;

[0067] S32: The foil obtained in step S31 is used as an anode, and the fixture is fixed in the corrosion tank and DC corrosion is carried out in a mixed acid of hydrochloric acid solution and sulfuric acid solution at a temperature of 355K and a volume ratio of 5:1 to obtain a perforated foil, wherein the concentration of the hydrochloric acid solution is 1.2 mol / L, the concentration of the sulfuric acid solution is 4.0 mol / L, and the average corrosion current density is 0.35 A / cm 2 , the corrosion time is 160s:

[0068] S33: Etching and expanding the hole: The perforated foil obtained in step S32 is subjected to secondary hole expansion etching in a 0.55 mol / L nitric acid solution at 350 K, with a corrosion current density of 0.20 A / cm 2 , the etching time was 300s. After hole expansion, the foil was immersed in deionized water for 40min and then dried;

[0069] S34: treating the corroded foil obtained in step S33 in a 5.5wt% nitric acid solution at 70°C for 3.5min, taking out the corroded foil, and drying it for later use.

[0070] Example 3

[0071] This embodiment is a third embodiment of a method for preparing a test device for etching foil using a clamp with adjustable tension and the same. The difference between this embodiment and the first embodiment is that the method for preparing a test device for etching foil in this embodiment uses the above-mentioned clamp with adjustable tension to adjust the tension of the etching foil, and specifically includes the following steps:

[0072] S1: Fixing the foil: Cut the high-pressure optical foil with a thickness of 130 μm, a purity greater than 99.99%, and a cubic texture greater than 95% into foils of a certain size of 9 cm×15 cm, fix one end of the foil between the first clamping plate 41 and the second clamp 42 through the first nut 432, and fix the other end of the foil on the clamp 51 through the second nut 522.

[0073] S2: Adjusting the tension of the foil: The movable clamping plate structure 5 is driven to move on the slide rail 2 by the driving structure 6. Specifically, the screw 61 is rotated to drive the clamping member 51 to move on the slide rail 2, thereby changing the distance between the fixed clamping plate structure 4 and the movable clamping plate structure 5. The tension at both ends of the foil can be calculated according to Hooke's law. In this embodiment, the moving distance of the movable clamping plate structure 5 of 0 to 50 mm corresponds to the tension of 0 to 250 kN at both ends of the foil, that is, the moving distance of the movable clamping plate structure 5 is 0, that is, the movable clamping plate structure 5 does not move. At this time, the tension at both ends of the foil is 0, and the foil is in a natural state without being subjected to force; and when the movable clamping plate structure 5 moves 50 mm away from the fixed clamping plate structure 4, the tension at both ends of the foil is 250 kN. When the moving distance of the movable clamping plate structure 5 away from the fixed clamping plate structure 4 is between 0 and 50 mm, the tension at both ends of the foil can be calculated according to Hooke's law.

[0074] In this embodiment, the tension is set to 0 kN, that is, no tension is provided at both ends of the aluminum foil.

[0075] S3: Corrosion treatment: The foil with tension adjusted in the above step S2 is corroded under laboratory conditions to obtain a corroded foil. The specific operation steps are as follows:

[0076] S31: the foil with tension adjusted in step S2 is immersed in a sodium hydroxide solution with a temperature of 318K and a concentration of 0.25mol / L for 3 minutes, and then immersed in a mixed acid of a hydrochloric acid solution and a sulfuric acid solution with a volume ratio of 1:1 at a temperature of 333K for 2 minutes to remove the surface oxide film and oil film, wherein the concentration of the hydrochloric acid solution is 1.0mol / L and the concentration of the sulfuric acid solution is 3.5mol / L, and then immersed in deionized water for standby use;

[0077] S32: The foil obtained in step S31 is used as an anode, and the fixture is fixed in the corrosion tank and DC corrosion is carried out in a mixed acid of hydrochloric acid solution and sulfuric acid solution at a temperature of 345K and a volume ratio of 1:1 to obtain a perforated foil, wherein the concentration of the hydrochloric acid solution is 1.0 mol / L, the concentration of the sulfuric acid solution is 3.5 mol / L, and the average corrosion current density is 0.3 A / cm 2 , the corrosion time is 150s:

[0078] S33: Etching and expanding the hole: The perforated foil obtained in step S32 is subjected to secondary hole expansion etching in a 0.5 mol / L nitric acid solution at 341 K, with a corrosion current density of 0.18 A / cm 2 , the etching time was 280s. After hole expansion, the foil was immersed in deionized water for 38min and then dried;

[0079] S34: treating the corroded foil obtained in step S33 in a 5.0wt% nitric acid solution at 65°C for 3.0min, taking out the corroded foil, and drying it for later use.

[0080] Example 4

[0081] This embodiment is Example 4 of a method for preparing a test device for etching foil using a clamp with adjustable tension and the same. The difference between this embodiment and Example 3 is that in the method for preparing a test device for etching foil in this embodiment, the foil tension is set to 5 kN in step S2, and the parameters in other steps remain unchanged.

[0082] Example 5

[0083] This embodiment is Example 5 of a method for preparing a test device for etching foil using a clamp with adjustable tension and the same. The difference between this embodiment and Example 3 is that in the method for preparing a test device for etching foil in this embodiment, the foil tension is set to 10 kN in step S2, and the parameters in other steps remain unchanged.

[0084] Example 6

[0085] This embodiment is Example 6 of a method for preparing a test device for etching foil using a clamp with adjustable tension and the same. The difference between this embodiment and Example 3 is that in the method for preparing a test device for etching foil in this embodiment, the foil tension is set to 15 kN in step S2, and the parameters in other steps remain unchanged.

[0086] Performance test example

[0087] The performance of the etched foils prepared in Examples 3 to 6 was tested. The etched foils were formed at 520V using the Japanese EIAJ standard procedure, and the specific capacitance (4263B) was tested using a digital LCR meter.

[0088] Specifically, in the chemical process, the etched foil is first boiled in boiling water for 5 minutes, and then 2 The voltage was increased to 520 V in a 12% boric acid solution at a constant current density, and then charged at 520 V for 15 min. After the primary charge, the aluminum foil was heat treated at 773 K for 2 min. After the heat treatment, it was charged at 520 V for 3 min.

[0089] The polarization curves of the pretreated corroded foil in a mixed acid solution of 1.0 mol / L HCl and 3.5 mol / L H2SO4 with a volume ratio of 1:1 were tested using an Autolab electrochemical workstation. The purge potential rate was 50 mV / s. For the transient potential curve, the average current density was 0.4 A / cm 2 The test was conducted. The test system used a three-electrode system, namely, a working electrode, a Pt counter electrode, and a saturated calomel electrode as a reference electrode. The microscopic morphology of the corrosion foil was characterized by SEM (JSM-6510LV); the cubic texture calculation was performed by scanning with a scanner and then black-and-white processing for statistics.

[0090] Table 1 Performance test results

[0091]

[0092] In Examples 3-6, the distance between the fixed clamping structure and the movable clamping structure can be changed by an adjustable tension clamp, thereby changing the tension at both ends of the aluminum foil. The preparation of corrosion foil products under adjustable tension conditions was realized in the laboratory, and the influence of tension on the microstructure and corrosion performance of corrosion foil was studied, and some meaningful results were obtained.

[0093] Compared with Example 3, in Examples 4-6, the tension at both ends of the aluminum foil is adjusted by spiral advancement of the screw. As the tension increases, the average crack size of the oxide film on the surface of the aluminum foil becomes significantly larger, and the cubic texture occupancy rate decreases. This is because as the foil is subjected to force in the horizontal direction, the aluminum foil is stretched to a certain extent, cracks appear on the surface aluminum oxide layer during the stretching process, and irregular deformation occurs in the cubic texture of the aluminum core layer.

[0094] Comparing the comprehensive performance of the electrode foil after corrosion, as the tensile tension increases, the bending strength of the electrode foil gradually decreases. When the tension is about 5kN, the electrostatic capacitance of the electrode foil reaches 0.875μF / cm 2 This is because appropriate and uniform surface defects are conducive to corrosion pores. When the tension is too large, the cracks in the aluminum oxide film on the surface of the aluminum foil increase, affecting the uniformity of the corrosion pores. The stretching causes severe thinning, and the specific volume of the corrosion foil is significantly reduced. The cracks caused by the stretching process have a certain size and density. Therefore, in the process of corrosion pores, moderate crack defects can provide corrosion sites, increase the number and uniformity of corrosion pores, and are beneficial to the improvement of electrostatic capacitance.

[0095] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the embodiments here. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the claims of the present invention.

Claims

1. A test preparation method for corrosion foil, characterized in that: A tension-adjustable clamp is used to adjust the tension of the corrosion foil, the clamp comprising a suspension frame (1), a slide rail (2), a support frame (3), a fixed clamping plate structure (4) for clamping one end of the aluminum foil (10), and a movable clamping plate structure (5) for clamping the other end of the aluminum foil (10); the slide rail (2) is connected between the suspension frame (1) and the support frame (3); the fixed clamping plate structure (4) is fixedly arranged on the suspension frame (1); the suspension frame (1) is provided with a through hole for the aluminum foil (10) to pass through; the movable clamping plate structure (5) is slidably arranged on the slide rail (2); the movable clamping plate structure (5) is also connected to a driving structure (6) for driving the movable clamping plate structure (5) to slide; The specific steps include: S1: Fixing the foil: Cut the high-pressure light foil into foils of required size, and then fix one end of the foil to the fixed clamping plate structure (4) and the other end to the movable clamping plate structure (5); S2: Adjusting the foil tension: The driving structure (6) drives the movable clamping plate structure (5) to move on the slide rail (2), thereby changing the distance between the fixed clamping plate structure (4) and the movable clamping plate structure (5), and calculating the tension at both ends of the foil according to Hooke's law; S3: Corrosion treatment: the foil with tension adjusted in step S2 is corroded under laboratory conditions to obtain a corroded foil; S31: the foil with tension adjusted in step S2 is immersed in a sodium hydroxide solution with a temperature of 310-330K and a concentration of 0.225-0.275 mol / L for 2.5-3.5 min, and then immersed in a mixed acid of a hydrochloric acid solution and a sulfuric acid solution with a volume ratio of (0.5-5):1 at a temperature of 320-345K for 1.5-2.5 min to remove the surface oxide film and oil film, wherein the concentration of the hydrochloric acid solution is 0.8-1.2 mol / L, and the concentration of the sulfuric acid solution is 3.0-4.0 mol / L, and then immersed in deionized water for standby use; S32: The foil obtained in step S31 is used as an anode, and a fixture is fixed in a corrosion tank and a porous foil is obtained by direct current corrosion in a mixed acid of a hydrochloric acid solution and a sulfuric acid solution at a temperature of 335-355K and a volume ratio of (0.5-5):1, wherein the concentration of the hydrochloric acid solution is 0.8-1.2 mol / L, the concentration of the sulfuric acid solution is 3.0-4.0 mol / L, and the average corrosion current density is 0.25-0.35 A / cm 2 , corrosion time is 140~160s: S33: Etching and expanding the hole: The perforated foil obtained in step S32 is subjected to secondary hole expansion corrosion in a 0.45-0.55 mol / L nitric acid solution at 330-350 K, with a corrosion current density of 0.15-0.20 A / cm 2 , the etching time is 250~300s. After hole expansion, the foil is immersed in deionized water for 35~40min and then dried; S34: treating the corroded foil obtained in step S33 in a nitric acid solution with a weight percentage of 4.5-5.5wt% for 2.5-3.5min at a temperature of 60-70°C, taking out the corroded foil, and drying it for later use.

2. The method for preparing a corrosion foil test according to claim 1, characterized in that: The thickness of the high-pressure light foil in step S1 is 115-145 μm, the purity is greater than 99.99%, and the cubic texture is greater than 95%.

3. The test preparation method of a corrosion foil according to claim 1, characterized in that: In the step S2, the moving distance of the movable clamping plate structure (5) is 0-50 mm, which corresponds to the tension of 0-250 kN on both ends of the foil.

4. The test preparation method of a corrosion foil according to claim 1, characterized in that: The fixing clamping plate structure (4) comprises a first clamping plate (41), a second clamping plate (42) and a first fixing assembly (43) for fixing the aluminum foil (10) between the first clamping plate (41) and the second clamping plate (42); the first clamping plate (41) and the second clamping plate (42) are arranged on the hanging frame (1); and the first fixing assembly (43) is arranged on the first clamping plate (41) and / or the second clamping plate (42).

5. The test preparation method of a corrosion foil according to claim 1, characterized in that: The movable clamping plate structure (5) comprises a clamping member (51) slidably connected to the slide rail (2) and a second fixing component (52) used for fixing the aluminum foil (10) on the clamping member (51); the second fixing component (52) is connected to the clamping member (51).

6. The test preparation method of a corrosion foil according to claim 5, characterized in that: The clamping member (51) is provided with a protrusion (53); the slide rail (2) is provided with a slide groove (21); and the slide groove (21) is slidably connected to the protrusion (53).

7. The test preparation method of a corrosion foil according to claim 5, characterized in that: The driving structure (6) comprises a screw rod (61) connected to the clamping member (51); and the support frame (3) is provided with a third threaded hole (31) threadably matched with the screw rod (61).

8. The test preparation method of a corrosion foil according to claim 7, characterized in that: The screw rod (61) is provided with scales; the spacing of the scales is 1-4 mm.

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