CN116426850B - Method for preparing high-cubic texture occupancy electronic aluminum foil based on microwave plasma sintering - Google Patents
Method for preparing high-cubic texture occupancy electronic aluminum foil based on microwave plasma sintering Download PDFInfo
- Publication number
- CN116426850B CN116426850B CN202310261192.0A CN202310261192A CN116426850B CN 116426850 B CN116426850 B CN 116426850B CN 202310261192 A CN202310261192 A CN 202310261192A CN 116426850 B CN116426850 B CN 116426850B
- Authority
- CN
- China
- Prior art keywords
- aluminum foil
- mixed gas
- microwave plasma
- rolling
- plasma sintering
- 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.)
- Active
Links
- 239000011888 foil Substances 0.000 title claims abstract description 109
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 97
- 238000005245 sintering Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 52
- 238000000137 annealing Methods 0.000 claims abstract description 24
- 238000005096 rolling process Methods 0.000 claims abstract description 17
- 238000005098 hot rolling Methods 0.000 claims abstract description 14
- 238000005097 cold rolling Methods 0.000 claims abstract description 12
- 238000005266 casting Methods 0.000 claims abstract description 9
- 238000003723 Smelting Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 51
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 13
- 230000001276 controlling effect Effects 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 11
- 230000001105 regulatory effect Effects 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 4
- 238000009749 continuous casting Methods 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000001681 protective effect Effects 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 7
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 17
- 239000003990 capacitor Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/40—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0226—Hot rolling
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0236—Cold rolling
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
-
- 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials 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 preparing high cubic texture occupancy electronic aluminum foil based on microwave plasma sintering, which is characterized in that after high-purity aluminum with purity of more than 99.99 percent is produced according to the process steps of smelting, casting, soaking, hot rolling, cold rolling, intermediate annealing, foil rolling and the like of the traditional electronic aluminum foil, the aluminum foil after the last foil rolling pass is subjected to microwave plasma sintering heat treatment in mixed gas which has the property of sintering auxiliary agent and contains reducing atmosphere and protective atmosphere, and finally the aluminum foil with high cubic texture occupancy is prepared, and the method has the advantages that: compared with the traditional annealing process at present, the occupancy of the cubic texture can be improved by 1-4%; and can promote product quality, can improve production efficiency by a wide margin simultaneously.
Description
[ field of technology ]
The invention relates to the technical field of manufacturing of medium-high voltage anode aluminum foils for aluminum electrolytic capacitors, in particular to a method for preparing an electronic aluminum foil with high cubic texture occupancy based on microwave plasma sintering.
[ background Art ]
The capacitor plays an important role in the electronic component industry, is one of essential electronic components essential for the development of the electronic industry, is widely applied to places such as blocking and passing, coupling, bypass, filtering, tuning loops and the like in a circuit, is mainly used in the fields such as consumer electronics, LEDs, 5G base stations and the like, and becomes one of important support posts of modern technology. The development of the capacitor industry has largely affected the development of the electronic information industry. In the electronic components used in the whole machine, the aluminum electrolytic capacitor accounts for more than 35% of the yield of four types of capacitors, and the electrode foil is the key raw material for manufacturing the aluminum electrolytic capacitor. The rapid development of the electronic industry, especially the rapid expansion of the market of the whole products such as communication products, computers, household appliances and the like, plays a role in promoting the development of the aluminum electrode foil industry. Meanwhile, as the requirements of miniaturization, high performance and sheet type of the aluminum electrolytic capacitor are more and more urgent, higher technical and quality requirements are also put forward for the manufacturing industry of the electrode foil, so that the market demand of the electrode foil is larger. The specific surface area of the aluminum foil is enlarged by electrochemical corrosion to increase the specific capacity of the current industrialized electrode foil, and the occupancy of the cubic texture in the aluminum foil directly determines the quality of the surface expansion effect after corrosion, so that the occupancy of the cubic texture in the aluminum foil is regarded as a key index of the manufacturing quality of the electrode foil at home and abroad, as the occupancy of the cubic texture of the current electrode foil for medium and high voltage is generally more than 95%.
Related researches exist at present, for example, chinese patent application 202010604197.5 discloses a finished product annealing method for improving the cubic texture of a high-voltage anode electronic aluminum foil, which comprises the steps of vacuumizing an annealing furnace, filling protective gas, heating to 450-550 ℃ for 5-10h, continuously heating to 580-650 ℃ for 14-18h, cooling to 520-570 ℃ for 5-10h, or enabling the material temperature to reach a set temperature, and finally cooling to the set temperature. For example, chinese patent application 200410023070.5 discloses a method for manufacturing a capacitor aluminum foil with a strong cubic texture, which mainly comprises smelting, casting blank, hot rolling, cold rolling and annealing of a finished product, and further comprises the steps of adopting an annealing method when the aluminum foil is cold rolled to a certain thickness X before the thickness of the finished product, and rolling to the thickness of the finished product through a smaller deformation degree.
The two patent applications can effectively weaken the influence of the unreasonable annealing temperature section on the opposite cube texture by regulating and controlling the final annealing process conditions, such as heating time, temperature section setting, heat preservation time and the like, thereby greatly improving the content of the cube texture and greatly improving the production efficiency. The current mature process flow for generating the electrode aluminum foil comprises the following steps: smelting, casting blank, hot rolling, cold rolling, intermediate annealing and finished product annealing. After the smelting control components are determined, the proportion of the cubic texture in the aluminum foil is influenced by the aluminum foil processing technology, and the most obvious influence is the finished product annealing technology.
[ invention ]
Aiming at the problems that finished product annealing of the anode electronic aluminum foil in the industry in the prior art is generally carried out in a protective gas annealing furnace with a vacuumizing function, but according to the current general finished product annealing process, the growth of the electronic aluminum foil cube texture is blocked and the occupancy of the final cube texture is influenced due to the fact that the heating time is long and the temperature section is set unreasonably, the invention provides a method for preparing the electronic aluminum foil with high cube texture occupancy based on microwave plasma sintering, which is proposed on the basis that the positive effect can be obtained by completely changing the annealing mode, and a better research result is obtained.
The aim of the invention is achieved by the following technical scheme:
microwave is a high-frequency electromagnetic wave with the frequency range of 0.3GHz-300GHz, and microwave heating is to convert microwave energy into heat energy by utilizing dielectric loss of dielectric medium in a high-frequency electric field. The microwave plasma heating is to generate plasma glow discharge by utilizing ionization of thin gas in a high-frequency electromagnetic field, and the plasma can absorb electromagnetic waves to convert microwave energy into heat energy. The solid medium in the microwave plasma device is bombarded with high strength microwave electric field to raise the temperature of the medium surface and is irradiated or transmitted with microwave to affect the physical and chemical properties of the medium. Therefore, microwaves are also an efficient rapid heating means.
A method for preparing high cube texture occupancy electronic aluminum foil based on microwave plasma sintering comprises the following steps:
1) Casting: smelting, preserving heat, refining and standing raw materials cast by high-purity molten aluminum, producing a slab ingot by semi-continuous casting, and rapidly cooling at a casting temperature of 685-720 ℃ to obtain a formed slab ingot;
2) Homogenizing: homogenizing the formed slab ingot obtained in the previous step through an annealing furnace at 550-610 ℃ for 15-40 hours, and cooling to room temperature after homogenizing;
3) And (3) hot rolling: carrying out hot rolling treatment on the slab ingot subjected to homogenization treatment in the previous step, wherein the hot rolling start temperature is 500-550 ℃, and the final rolling temperature is 220-350 ℃ to obtain a hot rolled coiled material with the hot rolling thickness of 5-7 mm;
4) Cold rolling: carrying out cold rolling treatment on the hot rolled coiled material obtained in the previous step, wherein the cold rolling speed is 200-600m/min, and obtaining a cold rolled coiled material with the intermediate thickness of 0.35-0.50 mm;
5) Foil rolling: foil rolling treatment is carried out on the cold rolled coiled material obtained in the previous step, the foil rolling speed is 200-600m/min, and the obtained aluminum foil with the thickness of 0.10-0.15mm is obtained;
6) Microwave plasma sintering: carrying out microwave plasma sintering heat treatment on the aluminum foil obtained in the step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 5-10 ℃/min, the heating temperature range to be 550-620 ℃ and the heat preservation time to be 5-10h, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with mole ratio of hydrogen to argon of 1 (1-10), or mixed gas with mole ratio of methane to argon of 1 (1-20).
In the invention, the following components are added:
the mixed gas in the step 6) is a combination with a reducing atmosphere and a protective atmosphere, wherein the combination has the property of a sintering aid.
Compared with the prior art, the invention has the following advantages:
1. the key technology of the method for preparing the electronic aluminum foil with high cubic texture occupancy based on microwave plasma sintering is that a microwave plasma heat treatment technology is adopted, the cubic texture occupancy of the aluminum foil is improved, the aluminum foil subjected to the final foil rolling pass is subjected to microwave plasma sintering heat treatment in mixed gas which has the property of sintering auxiliary agent and contains reducing atmosphere and protective atmosphere, and finally the aluminum foil with high cubic texture occupancy is prepared.
2. According to the method for preparing the electronic aluminum foil with high cubic texture occupancy based on microwave plasma sintering, the aluminum foil coil is subjected to microwave plasma heat treatment, and the influence of an unreasonable annealing temperature section on the production of the opposite cubic texture can be obviously weakened by reasonably setting the temperature section and the heating time and controlling the heating speed based on the high heating efficiency of microwave plasma, so that the content of the cubic texture is greatly improved, and meanwhile, the production efficiency is greatly improved.
[ description of the drawings ]
FIG. 1 is a schematic diagram of the microwave plasma heat treatment of the foil rolled in step 5) of example 1 in a tube furnace;
fig. 2 is an optical diagram of the effect of cubic texture pits on the surface of an annealed aluminum foil of an electronic aluminum foil with high cubic texture occupancy obtained in the example of the present invention and an annealed aluminum foil of an electronic aluminum foil obtained in the comparative example (fig. 2a, after conventional annealing of the comparative example; fig. 2b, example 1; fig. 2c, example 3; fig. 2d, example 5).
[ detailed description ] of the invention
The following describes the invention in more detail with reference to examples.
Example 1:
a method for preparing high cube texture occupancy electronic aluminum foil based on microwave plasma sintering comprises the following steps:
1) Casting: smelting, preserving heat, refining and standing raw materials cast by high-purity molten aluminum, producing a slab ingot by semi-continuous casting, and rapidly cooling at the casting temperature of 720 ℃ to obtain a formed slab ingot;
2) Homogenizing: homogenizing the formed slab ingot obtained in the previous step through an annealing furnace at the homogenizing temperature of 600 ℃ for 15 hours, and air-cooling to room temperature after homogenizing;
3) And (3) hot rolling: carrying out hot rolling treatment on the slab ingot subjected to homogenization treatment in the previous step, and obtaining a hot rolled coiled material with the hot rolled thickness of 7mm, wherein the hot rolling initial rolling temperature is 550 ℃ and the final rolling temperature is 250 ℃;
4) Cold rolling: carrying out cold rolling treatment on the hot rolled coiled material obtained in the previous step, wherein the cold rolling speed is 600m/min, and obtaining a cold rolled coiled material with the intermediate thickness of 0.35 mm;
5) Foil rolling: foil rolling treatment is carried out on the cold rolled coiled material obtained in the previous step, the foil rolling speed is 600m/min, and the obtained aluminum foil with the finished product thickness of 0.10mm-0.15mm is obtained;
6) Microwave plasma sintering: carrying out microwave plasma sintering heat treatment on the aluminum foil with the thickness of 0.12mm obtained in the previous step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 5 ℃/min, the heating temperature range to be 550 ℃, the heat preservation time to be 10 hours, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with a molar ratio of hydrogen to argon of 1:1.
FIG. 1 is a schematic view showing the microwave plasma heat treatment of an aluminum foil of 0.12mm thickness in a tube furnace according to example 1 of the present invention.
Example 2:
a method for preparing high cube texture occupancy electronic aluminum foil based on microwave plasma sintering comprises the following steps:
wherein:
step 6) carrying out microwave plasma sintering heat treatment on the aluminum foil with the thickness of 0.12mm obtained in the step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 6 ℃/min, the heating temperature range to be 560 ℃, the heat preservation time to be 9 hours, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with a molar ratio of hydrogen to argon of 1:5.
The other steps are the same as in example 1.
Example 3:
a method for preparing high cube texture occupancy electronic aluminum foil based on microwave plasma sintering comprises the following steps:
wherein:
step 6) carrying out microwave plasma sintering heat treatment on the aluminum foil with the thickness of 0.12mm obtained in the step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 7 ℃/min, the heating temperature range to be 580 ℃, the heat preservation time to be 7h, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with a molar ratio of hydrogen to argon of 1:10.
The other steps are the same as in example 1.
Example 4:
a method for preparing high cube texture occupancy electronic aluminum foil based on microwave plasma sintering comprises the following steps:
wherein:
step 6) carrying out microwave plasma sintering heat treatment on the aluminum foil with the thickness of 0.12mm obtained in the step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 7 ℃/min, the heating temperature range to be 580 ℃, the heat preservation time to be 8 hours, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with the molar ratio of methane to argon being 1:1.
The other steps are the same as in example 1.
Example 5:
a method for preparing high cube texture occupancy electronic aluminum foil based on microwave plasma sintering comprises the following steps:
wherein:
step 6) carrying out microwave plasma sintering heat treatment on the aluminum foil with the thickness of 0.12mm obtained in the step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 8 ℃/min, the heating temperature range to be 590 ℃, the heat preservation time to be 6 hours, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with the molar ratio of methane to argon being 1:10.
The other steps are the same as in example 1.
Example 6:
a method for preparing high cube texture occupancy electronic aluminum foil based on microwave plasma sintering comprises the following steps:
wherein:
step 6) carrying out microwave plasma sintering heat treatment on the aluminum foil with the thickness of 0.12mm obtained in the step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 5 ℃/min, the heating temperature range to be 560 ℃, the heat preservation time to be 10 hours, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with the molar ratio of methane to argon being 1:15.
The other steps are the same as in example 1.
Example 7:
a method for preparing high cube texture occupancy electronic aluminum foil based on microwave plasma sintering comprises the following steps:
wherein:
step 6) carrying out microwave plasma sintering heat treatment on the aluminum foil with the thickness of 0.12mm obtained in the step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 9 ℃/min, the heating temperature range to be 600 ℃, the heat preservation time to be 5 hours, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with the molar ratio of methane to argon being 1:20.
The other steps are the same as in example 1.
Example 8:
a method for preparing high cube texture occupancy electronic aluminum foil based on microwave plasma sintering comprises the following steps:
wherein:
step 6) carrying out microwave plasma sintering heat treatment on the aluminum foil with the thickness of 0.12mm obtained in the step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 10 ℃/min, the heating temperature range to be 620 ℃, the heat preservation time to be 5 hours, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with the molar ratio of methane to argon being 1:8.
The other steps are the same as in example 1.
Comparative example 1:
the aluminum foil with the thickness of 0.12mm obtained in the steps 1) to 5) above was treated by a conventional annealing process, and annealed in an argon-only protective atmosphere.
Comparative example 2:
step 6) the aluminum foil of 0.12mm thickness obtained in the above step was subjected to microwave plasma sintering heat treatment in air, lacking a mixed gas atmosphere, as compared with example 1.
Otherwise, the same as in example 1 was conducted.
FIG. 2 is an optical graph of the effect of cubic texture pits on the surface of an electronic aluminum foil with high cubic texture occupancy obtained in the example of the present invention and an annealed aluminum foil obtained in the comparative example (FIG. 2a: comparative example 1. Conventional annealing; FIG. 2b: example 1; FIG. 2c: example 3; FIG. 2d: example 5).
Comparative example 3:
step 6) the aluminum foil of 0.12mm thickness obtained in the above step was subjected to a microwave plasma sintering heat treatment in hydrogen gas, lacking a mixed gas atmosphere, as compared with example 1.
Otherwise, the same as in example 1 was conducted.
Comparative example 4:
step 6) the aluminum foil of 0.12mm thickness obtained in the above step was subjected to microwave plasma sintering heat treatment in methane, with the absence of a mixed gas atmosphere, as compared with example 1.
Otherwise, the same as in example 1 was conducted.
Experimental example:
the etching pit method is adopted to judge the occupancy of the cubic texture after the aluminum foil is annealed, and the etching solution is 0.6M HF+5M HNO 3 +0.8MAl 3+ The temperature is 30 ℃, the etching time is 10s, and the mixed solution is observed under an optical microscope after cleaning and drying. Table 1 is the cubic texture occupancy of the electronic aluminum foil with high cubic texture occupancy prepared in comparative examples and examples, see table 1:
table 1 cubic texture occupancy of electronic aluminum foil with high cubic texture occupancy prepared in comparative examples and examples
| Sample of | Thickness of aluminum foil | Occupancy of cubic texture |
| Comparative example 1 | 120μm | 94.2％ |
| Comparative example 2 | 120μm | 93.2％ |
| Comparative example 3 | 120μm | 94.6％ |
| Comparative example 4 | 120μm | 94.5％ |
| Example 1 | 120μm | 98.0％ |
| Example 2 | 120μm | 97.5％ |
| Example 3 | 120μm | 98.8％ |
| Example 4 | 120μm | 98.4％ |
| Example 5 | 120μm | 98.9％ |
| Example 6 | 120μm | 97.2％ |
| Example 7 | 120μm | 97.4％ |
| Example 8 | 120μm | 96.3％ |
1. As can be seen from a comparison of the examples and comparative example 1, the aluminum foil of 0.12mm thickness foil rolled in step 5) was subjected to the microwave plasma sintering heat treatment in a mixed gas having a reducing atmosphere and a protective atmosphere having a sintering aid property, and the cubic texture of the electronic aluminum foil having a high cubic texture occupancy obtained in the examples was 96.3 to 98.9%, which is 1.7 to 4.3% higher than that of the conventional annealing treated aluminum foil of comparative example 1.
2. From a comparison of examples and comparative examples 2 to 4, it can be seen that 0.12mm thick aluminum foil was subjected to microwave plasma sintering heat treatment in air, absent a mixed gas atmosphere: the lack of argon gas as protective atmosphere can lead to serious oxidization of aluminum foil in the microwave plasma sintering process, and under the condition of only argon gas protection, the lack of a small amount of hydrogen or methane and other gases with strong reducibility can not reduce a nanoscale oxide film naturally generated on the surface of the aluminum foil, and the existence of the oxide film can obstruct the microwave heating effect, so that the aluminum foil is heated unevenly, the difference between the bulk temperature and the actual measurement temperature is caused, and the electronic aluminum foil with high cubic texture occupancy rate can not be obtained.
The analytical reasons are: the argon is used as a protective atmosphere to prevent the aluminum foil from being oxidized in the microwave plasma sintering process, a small amount of hydrogen or methane is added to ionize the gases with strong reducibility under the plasma atmosphere to form an ionic state, the reduction of the aluminum oxide film with the nanometer thickness generated on the surface of the aluminum foil in the air is promoted, the aluminum foil is prevented from being heated unevenly and the difference between the bulk temperature and the measured temperature caused by the obstruction of the aluminum oxide film to microwaves, so that the aluminum foil added with a proper amount of reducing atmosphere can be fully subjected to uniform annealing, and the preferred orientation of the aluminum foil is improved.
The foregoing description is directed to the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the invention, and all equivalent changes or modifications made under the technical spirit of the present invention should be construed to fall within the scope of the present invention.
Claims (2)
1. A method for preparing high cubic texture occupancy electronic aluminum foil based on microwave plasma sintering is characterized by comprising the following steps: the method comprises the following steps:
1) Casting: smelting, preserving heat, refining and standing raw materials cast by high-purity molten aluminum, producing a slab ingot by semi-continuous casting, and rapidly cooling at a casting temperature of 685-720 ℃ to obtain a formed slab ingot;
2) Homogenizing: homogenizing the formed slab ingot obtained in the previous step through an annealing furnace at 550-610 ℃ for 15-40 hours, and cooling to room temperature after homogenizing;
3) And (3) hot rolling: carrying out hot rolling treatment on the slab ingot subjected to homogenization treatment in the previous step, wherein the hot rolling start temperature is 500-550 ℃, and the final rolling temperature is 220-350 ℃ to obtain a hot rolled coiled material with the hot rolling thickness of 5-7 mm;
4) Cold rolling: carrying out cold rolling treatment on the hot rolled coiled material obtained in the previous step, wherein the cold rolling speed is 200-600m/min, and obtaining a cold rolled coiled material with the intermediate thickness of 0.35-0.50 mm;
5) Foil rolling: foil rolling treatment is carried out on the cold rolled coiled material obtained in the previous step, the foil rolling speed is 200-600m/min, and the obtained aluminum foil with the thickness of 0.10-0.15mm is obtained;
6) Microwave plasma sintering: carrying out microwave plasma sintering heat treatment on the aluminum foil obtained in the step in mixed gas, regulating and controlling microwave power to enable the heating rate to be 5-10 ℃/min, the heating temperature range to be 550-620 ℃ and the heat preservation time to be 5-10h, and finally cooling to room temperature along with a furnace to obtain the electronic aluminum foil with the cubic texture occupancy rate higher than 95%;
the mixed gas is selected from mixed gas with mole ratio of hydrogen to argon of 1 (1-10), or mixed gas with mole ratio of methane to argon of 1 (1-20).
2. The method for preparing the high cube texture occupancy electronic aluminum foil based on microwave plasma sintering according to claim 1, wherein the method comprises the following steps: the mixed gas in the step 6) is selected from mixed gas with a molar ratio of hydrogen to argon of 1:1, mixed gas with a molar ratio of hydrogen to argon of 1:10, mixed gas with a molar ratio of methane to argon of 1:1, or mixed gas with a molar ratio of methane to argon of 1:10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310261192.0A CN116426850B (en) | 2023-03-17 | 2023-03-17 | Method for preparing high-cubic texture occupancy electronic aluminum foil based on microwave plasma sintering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310261192.0A CN116426850B (en) | 2023-03-17 | 2023-03-17 | Method for preparing high-cubic texture occupancy electronic aluminum foil based on microwave plasma sintering |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116426850A CN116426850A (en) | 2023-07-14 |
| CN116426850B true CN116426850B (en) | 2023-10-27 |
Family
ID=87082431
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310261192.0A Active CN116426850B (en) | 2023-03-17 | 2023-03-17 | Method for preparing high-cubic texture occupancy electronic aluminum foil based on microwave plasma sintering |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116426850B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06136495A (en) * | 1992-10-28 | 1994-05-17 | Showa Alum Corp | Production of aluminum material for electrolytic capacitor electrode |
| DE10057293C1 (en) * | 2000-11-17 | 2002-05-23 | Vaw Ver Aluminium Werke Ag | Production of an aluminum foil used as pharmaceutical blister packaging comprises cold rolling the foil using a roll stand, and plasma treating the metallic surface of the foil in a treating station before being coiled |
| CN111613446A (en) * | 2020-06-05 | 2020-09-01 | 南通海星电子股份有限公司 | Formation treatment method of high-water-resistance low-pressure aluminum foil |
| CN113026087A (en) * | 2021-04-29 | 2021-06-25 | 南通海星电子股份有限公司 | Preparation method of nano-microporous structure aluminum electrode foil for automobile electronics |
| CN113235023A (en) * | 2021-05-10 | 2021-08-10 | 广西正润新材料科技有限公司 | Low-voltage electronic aluminum foil for capacitor and preparation process thereof |
| CN113234907A (en) * | 2021-05-10 | 2021-08-10 | 广西正润新材料科技有限公司 | Medium-high voltage electronic aluminum foil for high-capacity high-strength capacitor and preparation method thereof |
| CN113235024A (en) * | 2021-05-10 | 2021-08-10 | 广西正润新材料科技有限公司 | Annealing method in production of medium-high voltage electronic aluminum foil for high-capacity high-strength capacitor |
-
2023
- 2023-03-17 CN CN202310261192.0A patent/CN116426850B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06136495A (en) * | 1992-10-28 | 1994-05-17 | Showa Alum Corp | Production of aluminum material for electrolytic capacitor electrode |
| DE10057293C1 (en) * | 2000-11-17 | 2002-05-23 | Vaw Ver Aluminium Werke Ag | Production of an aluminum foil used as pharmaceutical blister packaging comprises cold rolling the foil using a roll stand, and plasma treating the metallic surface of the foil in a treating station before being coiled |
| WO2002040189A1 (en) * | 2000-11-17 | 2002-05-23 | Vaw Aluminium Ag | Method and device for producing an aluminium film from an aluminium material |
| CN111613446A (en) * | 2020-06-05 | 2020-09-01 | 南通海星电子股份有限公司 | Formation treatment method of high-water-resistance low-pressure aluminum foil |
| CN113026087A (en) * | 2021-04-29 | 2021-06-25 | 南通海星电子股份有限公司 | Preparation method of nano-microporous structure aluminum electrode foil for automobile electronics |
| CN113235023A (en) * | 2021-05-10 | 2021-08-10 | 广西正润新材料科技有限公司 | Low-voltage electronic aluminum foil for capacitor and preparation process thereof |
| CN113234907A (en) * | 2021-05-10 | 2021-08-10 | 广西正润新材料科技有限公司 | Medium-high voltage electronic aluminum foil for high-capacity high-strength capacitor and preparation method thereof |
| CN113235024A (en) * | 2021-05-10 | 2021-08-10 | 广西正润新材料科技有限公司 | Annealing method in production of medium-high voltage electronic aluminum foil for high-capacity high-strength capacitor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116426850A (en) | 2023-07-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102812133B (en) | Process for producing grain-oriented magnetic steel sheet | |
| CN103834858B (en) | A kind of manufacture method of low iron loss non-orientation silicon steel | |
| RU2529258C1 (en) | Method to produce sheet from unoriented electrical steel | |
| EP2796571B1 (en) | High silicon steel sheet having excellent productivity and magnetic properties and method for manufacturing same | |
| CN105908021B (en) | A kind of capacitor fine aluminium Cathode Foil and its manufacture method | |
| CN113234907B (en) | Medium-high voltage electronic aluminum foil for high-capacity high-strength capacitor and preparation method thereof | |
| CN102851577A (en) | High grade non-oriented silicon steel produced by continuous casting and rolling of sheet billet and production method thereof | |
| CN113235023B (en) | Low-voltage electronic aluminum foil for capacitor and preparation process thereof | |
| CN109652627B (en) | Annealing processing technology for producing high-performance metal wire | |
| CN112582182B (en) | Aluminum foil for high-specific-capacitance capacitor cathode and preparation process thereof | |
| CN201265027Y (en) | Direct switch-on heating annealing apparatus of hot rolled plate | |
| CN116426850B (en) | Method for preparing high-cubic texture occupancy electronic aluminum foil based on microwave plasma sintering | |
| CN113319524B (en) | Manufacturing method for reducing iron loss of oriented silicon steel by laser scoring | |
| CN112981151B (en) | High-elastic thermal effect block Ti-Ni-based material and preparation method thereof | |
| CN110904397B (en) | Multi-stage annealing process of high-voltage anode aluminum foil for electrolytic capacitor | |
| CN110605398A (en) | Preparation method of lanthanum-micro-doped high-temperature molybdenum wire | |
| KR102133909B1 (en) | Grain oriented electrical steel sheet and method for manufacturing the same | |
| CN114774723B (en) | Battery aluminum foil with high mechanical property and high conductivity and production method thereof | |
| CN111180190A (en) | Method for improving magnetic property of sintered neodymium-iron-boron magnet | |
| CN111424163A (en) | Equipment and process for quickly realizing temperature transition of strip steel in continuous annealing furnace | |
| CN1240869C (en) | Annealing method of high voltage electronic aluminium foil product | |
| JP2002173748A (en) | Method for producing high purity aluminum foil | |
| CN112430778A (en) | Thin non-oriented electrical steel plate and manufacturing method thereof | |
| CN117282771B (en) | Preparation method of AgCu15/4J29 composite strip for electronic packaging | |
| CN111876701A (en) | Finished product annealing method for improving cubic texture of high-voltage anode electronic aluminum foil |
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 |