CN110904372A - Method for preventing coarse grains from appearing in corrosion formation of low-voltage electronic aluminum foil and low-voltage electronic aluminum foil prepared by method - Google Patents
Method for preventing coarse grains from appearing in corrosion formation of low-voltage electronic aluminum foil and low-voltage electronic aluminum foil prepared by method Download PDFInfo
- Publication number
- CN110904372A CN110904372A CN201911207540.6A CN201911207540A CN110904372A CN 110904372 A CN110904372 A CN 110904372A CN 201911207540 A CN201911207540 A CN 201911207540A CN 110904372 A CN110904372 A CN 110904372A
- Authority
- CN
- China
- Prior art keywords
- less
- low
- percent
- aluminum alloy
- aluminum foil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/12—Alloys based on aluminium with copper as the next major constituent
- C22C21/18—Alloys based on aluminium with copper as the next major constituent with zinc
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/043—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with silicon as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/057—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with copper as the next major constituent
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metal Rolling (AREA)
Abstract
The invention discloses a method for preventing coarse grains from appearing in corrosion formation of a low-voltage electronic aluminum foil and the low-voltage electronic aluminum foil prepared by the method. Smelting, slagging-off, smelting component analysis, refining, casting, surface milling, uniform heat treatment, hot rolling, cold foil rolling and annealing are sequentially carried out on a pure aluminum ingot, and a low-voltage electronic aluminum foil is obtained after annealing is completed; the low-voltage electronic aluminum foil comprises 0.0005-0.0035% of silicon, 0.0005-0.0025% of iron, 0.0015-0.0035% of copper, less than 0.0015% of manganese, less than 0.0010% of zinc, less than 0.0010% of titanium, less than 0.0010% of gallium, less than 0.0010% of boron, less than 0.0003% of lead, less than or equal to 0.0100% of the total and the balance of Al. The method effectively solves the problem of generating coarse grains of the low-voltage electronic aluminum foil, thereby avoiding the generation of the uneven phenomenon caused by the coarse grains formed after the low-voltage electronic aluminum foil is formed subsequently. The mechanical property is not fluctuated, and the stability is obviously improved.
Description
Technical Field
The invention belongs to the technical field of electronic material processing, particularly relates to an electronic aluminum foil for an electrolytic capacitor, and particularly relates to a method for preventing coarse grains from appearing in corrosion formation of a low-voltage electronic aluminum foil and the low-voltage electronic aluminum foil prepared by the method.
Background
With the rapid development of electronic information industries such as photovoltaics, frequency converters, LED illuminating lamps, charging piles, electric vehicles and the like, the demand for electrolytic capacitors is increasing, and the aluminum electrolytic capacitors are widely applied due to the excellent performances such as low price, stable performance and the like. With the expansion of the electrolytic capacitor, better requirements are put on the aspects of miniaturization, high specific volume, high strength and the like of the electrolytic capacitor.
The low-voltage electronic aluminum foil is a material for manufacturing an anode plate of a low-voltage electrolytic capacitor and is generally used for working voltage below 200 vf. The corrosion technology is adopted to form fluctuation on the surface of the aluminum foil so as to enlarge the surface area of the polar plate and greatly improve the specific capacitance, the conventional low-voltage electronic aluminum foil is expanded by adopting an alternating current corrosion mode, and the quality of the corrosion expansion effect is directly related to the grain size and the orientation in the aluminum foil. In order to further increase the flexibility of the low-voltage electronic aluminum foil in the hard state during the corrosion process, the low-voltage electronic aluminum foil is usually heated to 300-500 ℃ to promote recrystallization. In addition, in the heating process, due to rapid heating, recrystallization abnormally grows to generate coarse grains, the generation of the coarse grains causes the electronic aluminum foil to have a rugged phenomenon in a formation process (an oxide film applying process), the capacitor cannot be wound and used, the appearance is poor, and the requirement of customers cannot be met.
Disclosure of Invention
The invention aims at the technical problems that: the low-voltage electronic aluminum foil is in a hard state, when the specific volume of the low-voltage electronic aluminum foil is increased through a corrosion process in the prior art, in order to increase the flexibility of the hard electronic aluminum foil, recrystallization is usually promoted through heating treatment at 300-500 ℃, and abnormal growth can occur in the recrystallization due to rapid heating in the process, so that coarse grains are generated, and the performance and the using effect of the electronic aluminum foil are directly influenced. The problem of coarse grains generated during corrosion formation of the hard-state low-voltage electronic aluminum foil is not solved well.
In order to solve the problems, the invention provides a method for preventing coarse grains from appearing in corrosion formation of a low-voltage electronic aluminum foil and the low-voltage electronic aluminum foil prepared by the method. The method effectively solves the problem that coarse grains are generated when the low-pressure hard electronic aluminum foil is corroded, the obtained low-pressure electronic aluminum foil is free of the generation of the coarse grains, the mechanical property is free of fluctuation, and the stability is obviously improved.
The invention is realized by the following technical scheme
A method for preventing coarse grains from appearing in corrosion formation of a low-voltage electronic aluminum foil comprises the following steps: smelting, slagging-off, smelting component analysis, refining, casting, surface milling, uniform heat treatment, hot rolling, cold foil rolling and annealing are sequentially carried out on a pure aluminum ingot, and a low-voltage electronic aluminum foil is obtained after annealing is completed; and rolling the cold foil for 6-9 times during rolling, wherein the reduction rate of each time is 20-50%, the rolling force is 30-100 tons, and the front and rear tension is 10-50 MPa.
According to the method for preventing the coarse grains from appearing in the corrosion formation of the low-voltage electronic aluminum foil, the purity of the pure aluminum ingot is equal to or greater than 99.99%.
The method for preventing the coarse grains from appearing in the corrosion formation of the low-voltage electronic aluminum foil comprises the steps of smelting a pure aluminum ingot at the temperature of 720-760 ℃ for 2-5 hours; after smelting and slagging off, detecting the components of the molten aluminum alloy, and adding an aluminum alloy additive (the aluminum alloy additive is well-known aluminum copper, aluminum silicon or aluminum iron alloy), so that the components of the molten aluminum alloy are kept at 0.0005 to 0.0035 percent of silicon, 0.0005 to 0.0025 percent of iron, 0.0015 to 0.0035 percent of copper, less than 0.0015 percent of manganese, less than 0.0010 percent of zinc, less than 0.0010 percent of titanium, less than 0.0010 percent of gallium, less than 0.0010 percent of boron, less than 0.0003 percent of lead, less than or equal to 0.0100 percent of the total, and the balance of Al.
The method for preventing the coarse grains from appearing in the corrosion formation of the low-voltage electronic aluminum foil comprises the step of introducing argon into an aluminum alloy solution for refining, wherein the refining temperature is 720-760 ℃ and the refining time is 20-30 min.
The method for preventing the coarse grains from appearing in the corrosion formation of the low-voltage electronic aluminum foil is characterized in that the casting temperature is 700-730 ℃, and the casting speed is 45-65 mm/min; the milling amount of the large-surface single side during milling is more than or equal to 5mm, and the thickness of the aluminum alloy cast ingot after milling is 250-270 mm.
The method for preventing the coarse grains from appearing in the corrosion formation of the low-voltage electronic aluminum foil comprises the following steps of uniformly heat treating a milled aluminum alloy cast ingot in a soaking furnace in two stages, wherein the furnace gas constant temperature of the first stage is 550-610 ℃, and the aluminum alloy cast ingot is subjected to heat preservation for 5-15 hours at the temperature; after the first stage is finished, performing a second stage, wherein the constant temperature of furnace gas in the second stage is 510-570 ℃, and the temperature of the aluminum alloy cast ingot is kept for 3-10 hours at the temperature; and the temperature of the aluminum alloy ingot when the ingot is discharged is 510-560 ℃.
According to the method for preventing coarse grains from appearing in corrosion formation of the low-voltage electronic aluminum foil, the hot rolling passes of the aluminum alloy cast ingot are 12-18 passes, the reduction of each pass is 10-50%, the aluminum alloy cast ingot is rolled until the thickness of the aluminum alloy cast ingot is 4-9 mm, lubricating emulsion is used for lubricating and cooling in the hot rolling process, the concentration of the emulsion is 4-6%, and the pressure of the emulsion is controlled to be 0.3 +/-0.05 MPa; controlling the temperature of the aluminum alloy coil blank after hot rolling to be 200-400 ℃;
and carrying out cold foil rolling treatment after hot rolling, and lubricating and cooling by using rolling oil in the cold foil rolling process, wherein the temperature of the rolling oil is 20-50 ℃, and the cold foil is rolled until the thickness of the aluminum alloy rolling blank is less than 0.110 mm.
According to the method for preventing the coarse grains from appearing in the corrosion formation of the low-voltage electronic aluminum foil, the aluminum alloy rolled blank after cold foil rolling is placed in a protective atmosphere annealing furnace for annealing, the initial temperature of furnace gas is controlled to be 100-300 ℃, and when the temperature of the aluminum alloy rolled blank is 100-300 ℃, the temperature is kept for 5-15 hours. And discharging the furnace after heat preservation is finished, and controlling the temperature below 150 ℃ during discharging.
The low-voltage electronic aluminum foil is prepared by the method for preventing coarse grains from appearing in corrosion formation of the low-voltage electronic aluminum foil.
The low-voltage electronic aluminum foil comprises the following elements in percentage by mass: 0.0005 to 0.0035 percent of silicon, 0.0005 to 0.0025 percent of iron, 0.0015 to 0.0035 percent of copper, less than 0.0015 percent of manganese, less than 0.0010 percent of zinc, less than 0.0010 percent of titanium, less than 0.0010 percent of gallium, less than 0.0010 percent of boron, less than 0.0003 percent of lead, less than or equal to 0.0100 percent of the total, and the balance of Al.
Compared with the prior art, the invention has the following positive beneficial effects
According to the invention, the electronic aluminum foil with better controlled element components and contents is rolled for 6-9 times in the cold foil rolling process, the pass reduction is large, the rolling force is large, the oil temperature is controlled to be 20-50 ℃ in the rolling process, and the condition ensures that the crystal grains of the internal tissue of the aluminum plate after hot rolling can be thoroughly crushed without damaging the crystal grains;
according to the invention, finished product annealing is adopted, and primary recovery recrystallization is simultaneously carried out through annealing at 50-300 ℃ and stress release, so that abnormal growth of grains caused by recrystallization due to rapid heating is avoided when high-temperature flexible treatment is carried out in the downstream corrosion formation process, and the phenomenon of unevenness caused by coarse grains after subsequent formation is avoided;
the tensile strength of the aluminum foil prepared by the invention at room temperature is 50-120 MPa (the thickness of a finished material is below 0.110 mm), detection results show that no coarse abnormal crystal grains exist, the granularity is less than 0.100mm, the generation of coarse abnormal crystal grains is effectively avoided, and the problem of coarse abnormal crystal grains generated in the low-voltage hard electronic aluminum foil in the prior art is solved. The grain size of the low-pressure hard electronic aluminum foil produced in the prior art in corrosion formation can reach 1-100 mm, namely, coarse grains are generated, the grain size distribution is uneven, the grain size change range is large, the performance of the electronic aluminum foil is greatly influenced, the aluminum foil is subjected to thermal stress in corrosion formation to cause uneven surface, and the aluminum foil cannot be effectively wound in the subsequent assembly of a capacitor.
Drawings
FIG. 1 is a schematic view of a low-voltage electronic aluminum foil prepared by the present invention,
fig. 2 is a schematic view of a low-voltage electronic aluminum foil prepared by the prior art.
Detailed Description
The present invention will be described in more detail with reference to the following embodiments for understanding the technical solutions of the present invention, but the present invention is not limited to the scope of the present invention.
Example 1
A low-voltage electronic aluminum foil comprises the following elements in percentage by mass: 0.0015% of silicon, 0.0020% of iron, 0.0025% of copper, less than 0.0015% of manganese, less than 0.0010% of zinc, less than 0.0010% of titanium, less than 0.0010% of gallium, less than 0.0010% of boron, less than 0.0003% of lead, less than or equal to 0.0100% of the total and the balance of Al.
The preparation method of the low-voltage electronic aluminum foil is a method for preventing coarse grains from appearing in corrosion formation, and specifically comprises the following steps:
(1) smelting: smelting 10 tons of pure aluminum ingots (the purity is equal to or greater than 99.99%) at 720-760 ℃ for 2-3 hours to obtain an aluminum alloy molten liquid matrix, removing scum on the surface of the aluminum alloy molten liquid, sampling and analyzing chemical components of the aluminum alloy molten liquid matrix, and adding an aluminum alloy additive into the aluminum alloy molten liquid matrix according to the set chemical component requirement of the low-voltage electronic aluminum foil, so that the aluminum alloy molten liquid components are kept as 0.0015% of silicon, 0.0020% of iron, 0.0025% of copper, less than 0.0015% of manganese, less than 0.0010% of zinc, less than 0.0010% of titanium, less than 0.0010% of gallium, less than 0.0010% of boron, less than 0.0003% of lead, less than or equal to 0.0100; stirring by using electromagnetic stirring equipment to obtain an aluminum alloy melt with uniformly distributed alloy elements;
(2) refining the molten aluminum alloy: refining the aluminum alloy melt, namely introducing argon into the aluminum alloy melt for refining, wherein the refining temperature is controlled to be 720-760 ℃, and the refining time is 20-30 min; slagging off and standing after refining;
(3) casting: casting the refined aluminum alloy melt, wherein the casting temperature is controlled to be 700-730 ℃, and the casting speed is controlled to be 45-50 mm/min; finishing casting to obtain an aluminum alloy ingot;
(4) milling a surface: cutting the head and milling the aluminum alloy cast ingot obtained in the step (3), wherein the milling amount of the large surface on one side is more than or equal to 5 mm; the cast ingot surface is smooth without obvious knife lines after surface milling, and the thickness is 250 +/-1 mm after surface milling;
(5) uniform heat treatment: placing the aluminum alloy cast ingot subjected to surface milling in the step (4) into a soaking furnace to carry out two-stage heat treatment; the furnace gas constant temperature of the first stage is 550-610 ℃, and the aluminum alloy cast ingot is insulated for 5-6 hours at the temperature; after the first stage is finished, performing a second stage, wherein the constant temperature of furnace gas in the second stage is 510-570 ℃, and the temperature of the aluminum alloy cast ingot is kept for 3-4 hours at the temperature; discharging the aluminum alloy ingot after heat preservation, wherein the temperature of the aluminum alloy ingot during discharging is 510-560 ℃;
(6) hot rolling: carrying out hot rolling on the aluminum alloy ingot subjected to the uniform heat treatment in the step (5) for 12 passes, wherein the rolling reduction of each pass is 20-50%, and the aluminum alloy ingot is rolled until the thickness of the aluminum alloy ingot is 7 mm; lubricating emulsion is used for lubricating and cooling in the hot rolling process, the concentration of the emulsion is 4-6%, and the pressure of the emulsion is controlled to be 0.3 +/-0.05 MPa; controlling the temperature of the aluminum alloy coil blank to be 200 +/-50 ℃ after hot rolling;
(7) cold foil rolling: carrying out cold foil rolling on the aluminum alloy coil blank subjected to hot rolling in the step (6); rolling for 8 times, wherein the reduction rate of each time is 30-40%, the rolling force is 90 tons, and the tension before and after rolling is 20 MPa;
lubricating and cooling by using rolling oil in the cold foil rolling process, wherein the temperature of the rolling oil is 20-30 ℃, and the cold foil is rolled until the thickness of the aluminum alloy rolling blank is 0.060-0.105 mm;
(8) annealing: and (3) annealing the aluminum alloy rolled blank subjected to cold foil rolling in a nitrogen furnace (a protective atmosphere annealing furnace), controlling the initial temperature of furnace gas to be 100-150 ℃, and preserving the heat of the aluminum alloy rolled blank at the temperature for 15 hours. And (3) discharging the aluminum foil after heat preservation is finished, controlling the temperature below 150 ℃ during discharging, discharging the aluminum foil to obtain the low-voltage electronic aluminum foil, and performing corrosion observation (corrosion for 1-5 min) by using hydrochloric acid, nitric acid and hydrofluoric acid (well known by the technical personnel in the field), wherein the result is shown in figure 1.
Example 2
A low-voltage electronic aluminum foil comprises the following elements in percentage by mass: 0.0035 percent of silicon, 0.0025 percent of iron, 0.0030 percent of copper, less than 0.0015 percent of manganese, less than 0.0010 percent of zinc, less than 0.0010 percent of titanium, less than 0.0010 percent of gallium, less than 0.0010 percent of boron, less than 0.0003 percent of lead, less than or equal to 0.0100 percent of the total and the balance of Al.
The preparation method of the low-voltage electronic aluminum foil is a method for preventing coarse grains from appearing in corrosion formation, and specifically comprises the following steps:
(1) smelting: smelting 15 tons of pure aluminum ingots (the purity is equal to or greater than 99.99%) at 720-760 ℃ for 3-4 hours to obtain an aluminum alloy molten liquid matrix, skimming dross on the surface of the aluminum alloy molten liquid, sampling and analyzing the chemical components of the aluminum alloy molten liquid matrix, and adding an aluminum alloy additive into the aluminum alloy molten liquid matrix according to the set chemical component requirement of the low-voltage electronic aluminum foil, so that the components of the aluminum alloy molten liquid are kept as 0.0035% of silicon, 0.0025% of iron, 0.0030% of copper, less than 0.0015% of manganese, less than 0.0010% of zinc, less than 0.0010% of titanium, less than 0.0010% of gallium, less than 0.0010% of boron, less than 0.0003% of lead, less than or equal to; stirring by using electromagnetic stirring equipment to obtain an aluminum alloy melt with uniformly distributed alloy elements;
(2) refining the molten aluminum alloy: refining the aluminum alloy melt, namely introducing argon into the aluminum alloy melt for refining, wherein the refining temperature is controlled to be 730-760 ℃, and the refining time is 20-30 minutes; slagging off and standing after refining;
(3) casting: casting the refined aluminum alloy melt, wherein the casting temperature is controlled to be 700-730 ℃, and the casting speed is controlled to be 50-55 mm/min; finishing casting to obtain an aluminum alloy ingot;
(4) milling a surface: cutting the head and milling the aluminum alloy cast ingot obtained in the step (3), wherein the milling amount of the large surface on one side is more than or equal to 5 mm; the cast ingot surface is smooth without obvious knife lines after surface milling, and the thickness is 260 +/-1 mm after surface milling;
(5) uniform heat treatment: placing the aluminum alloy cast ingot subjected to surface milling in the step (4) into a soaking furnace to carry out two-stage heat treatment; the furnace gas constant temperature of the first stage is 550-610 ℃, and the aluminum alloy cast ingot is insulated for 8-9 hours at the temperature; after the first stage is finished, performing a second stage, wherein the constant temperature of furnace gas in the second stage is 510-570 ℃, and the temperature of the aluminum alloy cast ingot is kept for 4-5 hours at the temperature; discharging the aluminum alloy ingot after heat preservation, wherein the temperature of the aluminum alloy ingot during discharging is 510-560 ℃;
(6) hot rolling: carrying out hot rolling on the aluminum alloy ingot subjected to the uniform heat treatment in the step (5) for 15 times, wherein the reduction of each time is 20-50%, and the aluminum alloy ingot is rolled until the thickness of the aluminum alloy ingot is 6 mm; lubricating emulsion is used for lubricating and cooling in the hot rolling process, the concentration of the emulsion is 4-6%, and the pressure of the emulsion is controlled to be 0.3 +/-0.05 MPa; controlling the temperature of the aluminum alloy coil blank to be 300 +/-50 ℃ after hot rolling;
(7) cold foil rolling: carrying out cold foil rolling on the aluminum alloy coil blank subjected to hot rolling in the step (6); rolling for 7 passes, wherein the reduction rate of each pass is 20-30%, the rolling force is 70 tons, and the tension before and after rolling is 30 MPa;
lubricating and cooling by using rolling oil in the cold foil rolling process, wherein the temperature of the rolling oil is 30-40 ℃, and cold foil rolling is carried out until the thickness of an aluminum alloy rolling blank is 0.060-0.105 mm;
(8) annealing: and (3) annealing the aluminum alloy rolled blank subjected to cold foil rolling in a nitrogen furnace (a protective atmosphere annealing furnace), controlling the initial temperature of furnace gas to be 150-200 ℃, and preserving the heat of the aluminum alloy rolled blank at the temperature for 10 hours. And discharging the aluminum foil after heat preservation is finished, controlling the temperature below 150 ℃ during discharging, and discharging to obtain the low-voltage electronic aluminum foil. The results of the corrosion observation (corrosion for 1-5 min) using hydrochloric acid + nitric acid + hydrofluoric acid (well known to those skilled in the art) are shown in FIG. 1.
Example 3
A low-voltage electronic aluminum foil comprises the following elements in percentage by mass: 0.0025% of silicon, 0.0015% of iron, 0.0020% of copper, less than 0.0015% of manganese, less than 0.0010% of zinc, less than 0.0010% of titanium, less than 0.0010% of gallium, less than 0.0010% of boron, less than 0.0003% of lead, less than or equal to 0.0100% of the total and the balance of Al.
The preparation method of the low-voltage electronic aluminum foil is a method for preventing coarse grains from appearing in corrosion formation, and specifically comprises the following steps:
(1) smelting: smelting 20 tons of pure aluminum ingots (the purity is equal to or greater than 99.99%) at 720-750 ℃ for 4-5 hours to obtain an aluminum alloy molten liquid matrix, removing scum on the surface of the aluminum alloy molten liquid, sampling and analyzing chemical components of the aluminum alloy molten liquid matrix, and adding an aluminum alloy additive into the aluminum alloy molten liquid matrix according to the set chemical component requirement of the low-voltage electronic aluminum foil, so that the components of the aluminum alloy molten liquid are kept as 0.0025% of silicon, 0.0015% of iron, 0.0020% of copper, less than 0.0015% of manganese, less than 0.0010% of zinc, less than 0.0010% of titanium, less than 0.0010% of gallium, less than 0.0010% of boron, less than 0.0003% of lead, less than or equal to 0.; stirring by using electromagnetic stirring equipment to obtain an aluminum alloy melt with uniformly distributed alloy elements;
(2) refining the molten aluminum alloy: refining the aluminum alloy melt, namely introducing argon into the aluminum alloy melt for refining, wherein the refining temperature is controlled to be 720-750 ℃, and the refining time is 20-30 minutes; slagging off and standing after refining;
(3) casting: casting the refined aluminum alloy melt, wherein the casting temperature is controlled to be 700-730 ℃, and the casting speed is controlled to be 60-65 mm/min; finishing casting to obtain an aluminum alloy ingot;
(4) milling a surface: cutting the head and milling the aluminum alloy cast ingot obtained in the step (3), wherein the milling amount of the large surface on one side is more than or equal to 5 mm; the cast ingot surface is smooth without obvious knife lines after surface milling, and the thickness is 270 +/-1 mm after surface milling;
(5) uniform heat treatment: placing the aluminum alloy cast ingot subjected to surface milling in the step (4) into a soaking furnace to carry out two-stage heat treatment; the furnace gas constant temperature of the first stage is 550-610 ℃, and the aluminum alloy cast ingot is insulated for 10-12 hours at the temperature; after the first stage is finished, performing a second stage, wherein the constant temperature of furnace gas in the second stage is 510-570 ℃, and the temperature of the aluminum alloy cast ingot is kept for 6-7 hours at the temperature; discharging the aluminum alloy ingot after heat preservation, wherein the temperature of the aluminum alloy ingot during discharging is 510-560 ℃;
(6) hot rolling: carrying out hot rolling on the aluminum alloy ingot subjected to the uniform heat treatment in the step (5) for 18 passes, wherein the reduction of each pass is 10-50%, and rolling is carried out until the thickness of the aluminum alloy ingot is 4 mm; lubricating emulsion is used for lubricating and cooling in the hot rolling process, the concentration of the emulsion is 4-6%, and the pressure of the emulsion is controlled to be 0.3 +/-0.05 MPa; controlling the temperature of the aluminum alloy coil blank to be 360-400 ℃ after hot rolling;
(7) cold foil rolling: carrying out cold foil rolling on the aluminum alloy coil blank subjected to hot rolling in the step (6); rolling for 6 times, wherein the reduction rate of each time is 40-50%, the rolling force is 40 tons, and the tension before and after rolling is 35-50 MPa;
lubricating and cooling by using rolling oil in the cold foil rolling process, wherein the temperature of the rolling oil is 40-50 ℃, and the cold foil is rolled until the thickness of the aluminum alloy rolling blank is 0.060-0.105 mm;
(8) annealing: and (3) annealing the cold foil rolled aluminum alloy roll blank in a nitrogen furnace (a protective atmosphere annealing furnace), controlling the initial temperature of furnace gas to be 200-250 ℃, and preserving the heat of the aluminum alloy roll blank at the temperature for 6 hours. And discharging the aluminum foil after heat preservation is finished, controlling the temperature below 150 ℃ during discharging, and discharging to obtain the low-voltage electronic aluminum foil. The results of the corrosion observation (corrosion for 1-5 min) using hydrochloric acid + nitric acid + hydrofluoric acid (well known to those skilled in the art) are shown in FIG. 1.
Fig. 1 is a schematic view of a low-voltage electronic aluminum foil prepared according to the present invention (grain size ≦ 1mm), and fig. 2 is a schematic view of a low-voltage electronic aluminum foil prepared according to the prior art (grain size 2-500 mm). As can be seen from fig. 1 and 2, the low-voltage electronic aluminum foil prepared by the present invention is significantly superior to the low-voltage electronic aluminum foil prepared by the prior art.
Claims (10)
1. A method for preventing coarse grains from appearing in corrosion formation of a low-voltage electronic aluminum foil is characterized by comprising the following steps: smelting, slagging-off, smelting component analysis, refining, casting, surface milling, uniform heat treatment, hot rolling, cold foil rolling and annealing are sequentially carried out on a pure aluminum ingot, and a low-voltage electronic aluminum foil is obtained after annealing is completed;
and rolling the cold foil for 6-9 times during rolling, wherein the reduction rate of each time is 20-50%, the rolling force is 30-100 tons, and the tension is 10-50 MPa.
2. The method for preventing coarse grains from occurring in the corrosion formation of the low-voltage electronic aluminum foil according to claim 1, wherein the purity of the pure aluminum ingot is ≧ 99.99%.
3. The method for preventing the occurrence of coarse grains in the corrosion formation of the low-voltage electronic aluminum foil according to claim 1, wherein the melting temperature of the pure aluminum ingot is 720-760 ℃, and the melting time is 2-5 hours;
after smelting and slagging off, detecting the components and adding aluminum alloy additives to ensure that the components of molten aluminum alloy are kept to be 0.0005-0.0035 percent of silicon, 0.0005-0.0025 percent of iron, 0.0015-0.0035 percent of copper, less than 0.0015 percent of manganese, less than 0.0010 percent of zinc, less than 0.0010 percent of titanium, less than 0.0010 percent of gallium, less than 0.0010 percent of boron, less than 0.0003 percent of lead, less than or equal to 0.0100 percent in total and the balance of Al.
4. The method for preventing the occurrence of coarse grains in the corrosion formation of the low-voltage electronic aluminum foil as recited in claim 1, wherein the refining is performed by introducing argon gas into the aluminum alloy solution, and the refining temperature is 720-760 ℃ and the refining time is 20-30 min.
5. The method for preventing coarse grains from occurring in the corrosion formation of the low-voltage electronic aluminum foil according to claim 1, wherein the temperature during casting is 700-730 ℃, and the casting speed is 45-65 mm/min; the milling amount of the large-surface single side during milling is more than or equal to 5mm, and the thickness of the aluminum alloy cast ingot after milling is 250-270 mm.
6. The method for preventing the occurrence of coarse grains in the corrosion formation of the low-voltage electronic aluminum foil according to claim 1, wherein the uniform heat treatment is a two-stage heat treatment in which the milled aluminum alloy ingot is placed in a soaking furnace, the temperature of the furnace gas in the first stage is 550-610 ℃, and the aluminum alloy ingot is kept at the temperature for 5-15 hours; after the first stage is finished, performing a second stage, wherein the constant temperature of furnace gas in the second stage is 510-570 ℃, and the temperature of the aluminum alloy cast ingot is kept for 3-10 hours at the temperature; and the temperature of the aluminum alloy ingot when the ingot is discharged is 510-560 ℃.
7. The method for preventing the coarse grains from appearing in the corrosion formation of the low-voltage electronic aluminum foil according to claim 1, wherein the aluminum alloy ingot is subjected to hot rolling for 12-18 passes, the reduction of each pass is 10% -50%, the aluminum alloy ingot is rolled until the thickness of the aluminum alloy ingot is 4-9 mm, lubricating emulsion is used for lubricating and cooling in the hot rolling process, the concentration of the emulsion is 4-6%, and the pressure of the emulsion is controlled to be 0.3 +/-0.05 MPa; controlling the temperature of the aluminum alloy coil blank after hot rolling to be 200-400 ℃;
and carrying out cold foil rolling treatment after hot rolling, and lubricating and cooling by using rolling oil in the cold foil rolling process, wherein the temperature of the rolling oil is 20-50 ℃, and the cold foil is rolled until the thickness of the aluminum alloy cast ingot is less than 0.110 mm.
8. The method for preventing coarse grains from occurring in the corrosion formation of the low-voltage electronic aluminum foil as recited in claim 1, wherein the aluminum alloy rolled blank after cold foil rolling is placed in a protective atmosphere annealing furnace for annealing, wherein the initial temperature of the furnace gas is controlled to be 100-300 ℃, and the temperature of the aluminum alloy rolled blank is kept for 5-15 hours at 100-300 ℃. And discharging the furnace after heat preservation is finished, and controlling the temperature below 150 ℃ during discharging.
9. The low-voltage electronic aluminum foil prepared by the method for preventing coarse grains from occurring in corrosion formation of the low-voltage electronic aluminum foil according to any one of claims 1 to 8.
10. The low-voltage electronic aluminum foil as claimed in claim 9, wherein the electronic aluminum foil comprises the following elements in percentage by mass:
0.0005 to 0.0035 percent of silicon, 0.0005 to 0.0025 percent of iron, 0.0015 to 0.0035 percent of copper, less than 0.0015 percent of manganese, less than 0.0010 percent of zinc, less than 0.0010 percent of titanium, less than 0.0010 percent of gallium, less than 0.0010 percent of boron, less than 0.0003 percent of lead, less than or equal to 0.0100 percent of the total, and the balance of Al.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911207540.6A CN110904372B (en) | 2019-11-30 | 2019-11-30 | Method for preventing coarse grains from appearing in corrosion formation of low-voltage electronic aluminum foil and low-voltage electronic aluminum foil prepared by method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911207540.6A CN110904372B (en) | 2019-11-30 | 2019-11-30 | Method for preventing coarse grains from appearing in corrosion formation of low-voltage electronic aluminum foil and low-voltage electronic aluminum foil prepared by method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110904372A true CN110904372A (en) | 2020-03-24 |
| CN110904372B CN110904372B (en) | 2020-12-08 |
Family
ID=69821087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911207540.6A Active CN110904372B (en) | 2019-11-30 | 2019-11-30 | Method for preventing coarse grains from appearing in corrosion formation of low-voltage electronic aluminum foil and low-voltage electronic aluminum foil prepared by method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110904372B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1341765A (en) * | 2001-09-06 | 2002-03-27 | 北京南辰秀普金属材料研究所 | Production process of aluminium foil for high-voltage anode of electrolytic capacitor |
| JP2002151362A (en) * | 2000-11-09 | 2002-05-24 | Nippon Foil Mfg Co Ltd | Aluminum alloy foil for electrolytic capacitor anode for low voltage, and method for manufacturing the same |
| JP2007046093A (en) * | 2005-08-09 | 2007-02-22 | Mitsubishi Alum Co Ltd | Aluminum foil for electrolytic capacitor electrode, and manufacturing method therefor |
| CN102787259A (en) * | 2012-07-12 | 2012-11-21 | 苏州有色金属研究院有限公司 | Aluminium alloy foil for lithium ion battery positive current collector and manufacturing method thereof |
| CN107492450A (en) * | 2017-08-09 | 2017-12-19 | 乳源东阳光优艾希杰精箔有限公司 | A kind of soft state aluminium foil of aluminium electrolutic capacitor low-voltage anode use and its manufacture method |
-
2019
- 2019-11-30 CN CN201911207540.6A patent/CN110904372B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002151362A (en) * | 2000-11-09 | 2002-05-24 | Nippon Foil Mfg Co Ltd | Aluminum alloy foil for electrolytic capacitor anode for low voltage, and method for manufacturing the same |
| CN1341765A (en) * | 2001-09-06 | 2002-03-27 | 北京南辰秀普金属材料研究所 | Production process of aluminium foil for high-voltage anode of electrolytic capacitor |
| JP2007046093A (en) * | 2005-08-09 | 2007-02-22 | Mitsubishi Alum Co Ltd | Aluminum foil for electrolytic capacitor electrode, and manufacturing method therefor |
| CN102787259A (en) * | 2012-07-12 | 2012-11-21 | 苏州有色金属研究院有限公司 | Aluminium alloy foil for lithium ion battery positive current collector and manufacturing method thereof |
| CN107492450A (en) * | 2017-08-09 | 2017-12-19 | 乳源东阳光优艾希杰精箔有限公司 | A kind of soft state aluminium foil of aluminium electrolutic capacitor low-voltage anode use and its manufacture method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110904372B (en) | 2020-12-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108315606B (en) | 1100 alloy aluminum foil for lithium battery and manufacturing method thereof | |
| CN106811628B (en) | A kind of method of casting and roll process production power battery case aluminium strip | |
| JP7033664B2 (en) | Manufacturing method of 1XXX cathode foil for aluminum electrolytic capacitors | |
| CN112831692B (en) | Aluminum-manganese alloy strip and preparation method thereof | |
| CN107492450B (en) | Soft aluminum foil for low-voltage anode of aluminum electrolytic capacitor and manufacturing method thereof | |
| JP5495649B2 (en) | Aluminum alloy foil for lithium ion secondary battery and method for producing the same | |
| WO2012169570A1 (en) | Aluminum alloy foil and method for manufacturing same | |
| CN102286714A (en) | Preparation method of copper-nickel-tin alloy | |
| WO2023050860A1 (en) | Multi-component precision high-resistance alloy with high strength and toughness, and preparation method therefor | |
| CN101789314B (en) | Aluminum foil for low-voltage electrolytic capacitor anode and production method thereof | |
| CN103290285A (en) | Magnesium-zinc-manganese-tin-yttrium alloy and preparation method of same | |
| JPH0790520A (en) | Production of high-strength cu alloy sheet bar | |
| CN110904372B (en) | Method for preventing coarse grains from appearing in corrosion formation of low-voltage electronic aluminum foil and low-voltage electronic aluminum foil prepared by method | |
| CN101792875B (en) | Aluminum foil and production method thereof | |
| CN101877278B (en) | Aluminum foil for medium-voltage electrolytic capacitor anode and method for producing same | |
| CN113385537A (en) | Method for directly cold rolling stainless steel without annealing | |
| JP4869398B2 (en) | Pure copper plate manufacturing method and pure copper plate | |
| CN110938768B (en) | High-voltage electronic aluminum foil without generation of coarse grains and preparation method thereof | |
| CN100475435C (en) | Method for preparing novel PS forme base | |
| CN112170484B (en) | Preparation method of copper-magnesium alloy strip for automobile relay | |
| CN113337760B (en) | Method for improving O-state conductivity of 5754 alloy | |
| CN114717445A (en) | Copper alloy and preparation method thereof | |
| CN110964935A (en) | Manufacturing method of aluminum material with good corrosion resistance for new energy automobile circuit board | |
| CN110964950A (en) | Manufacturing method of aluminum material for automobile heat insulation sheet | |
| CN114783778B (en) | Anode foil for medium-high voltage aluminum electrolytic capacitor and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |