CN111057978A - Preparation method of ultrafine-grained high-toughness heat-resistant aluminum alloy wire - Google Patents
Preparation method of ultrafine-grained high-toughness heat-resistant aluminum alloy wire Download PDFInfo
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- CN111057978A CN111057978A CN202010028492.0A CN202010028492A CN111057978A CN 111057978 A CN111057978 A CN 111057978A CN 202010028492 A CN202010028492 A CN 202010028492A CN 111057978 A CN111057978 A CN 111057978A
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 61
- 239000000956 alloy Substances 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 36
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 31
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000007670 refining Methods 0.000 claims abstract description 18
- 238000005266 casting Methods 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000005728 strengthening Methods 0.000 claims abstract description 13
- 238000003723 Smelting Methods 0.000 claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000010274 multidirectional forging Methods 0.000 claims abstract description 12
- 238000005096 rolling process Methods 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 239000003607 modifier Substances 0.000 claims abstract description 10
- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- -1 aluminum-erbium Chemical compound 0.000 claims abstract description 8
- ZGUQGPFMMTZGBQ-UHFFFAOYSA-N [Al].[Al].[Zr] Chemical compound [Al].[Al].[Zr] ZGUQGPFMMTZGBQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- WPPDFTBPZNZZRP-UHFFFAOYSA-N aluminum copper Chemical compound [Al].[Cu] WPPDFTBPZNZZRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000006698 induction Effects 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000000265 homogenisation Methods 0.000 claims abstract description 5
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 4
- 229910001371 Er alloy Inorganic materials 0.000 claims abstract description 4
- 229910001093 Zr alloy Inorganic materials 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims description 16
- 238000001125 extrusion Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 239000010949 copper Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 5
- 235000011089 carbon dioxide Nutrition 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 5
- 230000008023 solidification Effects 0.000 claims description 5
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000006104 solid solution Substances 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000013459 approach Methods 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000007712 rapid solidification Methods 0.000 claims description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 230000035882 stress Effects 0.000 description 7
- 239000004020 conductor Substances 0.000 description 6
- 239000000155 melt Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- 230000032683 aging Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910000676 Si alloy Inorganic materials 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018580 Al—Zr Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920001410 Microfiber Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- QQHSIRTYSFLSRM-UHFFFAOYSA-N alumanylidynechromium Chemical compound [Al].[Cr] QQHSIRTYSFLSRM-UHFFFAOYSA-N 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
A preparation method of a superfine-grain high-strength-toughness heat-resistant aluminum alloy wire comprises the following steps: (1) preparing materials: the composition comprises the following components in parts by weight: 100 parts of industrial pure aluminum, 0.7 part of aluminum-zirconium alloy, 0.4 part of aluminum-copper alloy, 0.4 part of aluminum-erbium alloy, 0.0015 part of refiner Al-5Ti-B, 0.06 part of modifier Sr and 0.5 part of refiner hexachloroethane; (2) smelting: adding pure aluminum into a coreless medium-frequency induction furnace, raising the furnace temperature to 740 ℃, starting ultrasonic vibration for 20s when the temperature reaches 720 ℃, after the metal is completely melted, adding an intermediate alloy, a modifier and a refiner by a bell jar pressing method, carrying out electromagnetic stirring during the process, and then starting refining and slagging off; (3) casting the prepared alloy liquid into ingots, and then carrying out multidirectional forging, homogenization treatment, rolling, stress relief annealing, low-temperature continuous ECAP, precipitation strengthening, drawing and twisting on the alloy ingots.
Description
Technical Field
The invention relates to a preparation technology of an aluminum alloy wire, in particular to a preparation technology of an ultra-fine grain, high-strength and high-toughness heat-resistant aluminum alloy wire.
Background
Chinese patent 201710083834.7 discloses a high-hardness aluminum alloy conductor, which is mainly prepared by mixing and smelting a plurality of metals, casting and rolling, so that the hardness of the material can be improved, but the influence of high alloying on the conductivity of the material is large; chinese patent 201810225926.9 discloses an aluminum alloy wire material, which is prepared by adding metal oxides such as magnesium oxide, zinc oxide, aluminum oxide, etc. to enhance the wear resistance and high temperature resistance of the aluminum alloy wire, but the metal oxides are difficult to be added into the aluminum alloy melting liquid, and the conductivity of the material is also seriously affected because the metal oxides are not conductive.
Chinese patent 201710266987.5 discloses a high-strength graphene rare earth aluminum alloy wire, wherein up to 14 alloy elements are added in addition to graphene and aluminum base, and since graphene is very easy to oxidize when added into molten metal and is difficult to dissolve in alloy, the requirements on melting equipment and melting process are very high, but how to add graphene into molten aluminum is not explained in the invention, and the processing process after melting is not explained.
Chinese patent 201610179825.3 discloses a method for preparing a high-conductivity heat-resistant aluminum alloy conductor, the aluminum liquid in the method is directly solidified by a launder, impurities are easily mixed in the casting process, and the tissue uniformity and density of the material cannot be guaranteed, so that the material prepared by the method cannot be guaranteed to have good performance. The method adopts a conventional ECAP method, and cannot eliminate negative effects caused by temperature rise in the deformation process.
Chinese patent 201410512562.4 discloses a method for improving the conductivity of aluminum-silicon alloy, and in principle, the higher the purity of the conductive material is, the better the conductivity of pure aluminum is, so the conductivity of pure aluminum is higher than that of aluminum alloy. The higher the alloying, the worse the conductivity of the material. The method adopts aluminum-copper intermediate alloy, aluminum-silicon intermediate alloy, aluminum-magnesium intermediate alloy, aluminum-zirconium intermediate alloy and aluminum-chromium intermediate alloy to be placed in a crucible resistance furnace for melting, so that the material can have certain strength, but the conductivity of the material can be greatly reduced. Actually, the conductivity of the aluminum-silicon alloy is only improved, and the universality is not high. In addition, the method adopts resistance furnace smelting, which causes uneven temperature rise, higher impurity content in the alloy and difficult guarantee of the purity of the alloy.
Disclosure of Invention
The invention aims to provide a preparation method of an ultra-fine grain high-toughness heat-resistant aluminum alloy wire.
The invention relates to a preparation method of a superfine-grain high-strength-toughness heat-resistant aluminum alloy wire, which comprises the following steps:
(1) preparing materials: the composition comprises the following components in parts by weight: 100 parts of industrial pure aluminum, 0.7 part of aluminum-zirconium alloy, 0.4 part of aluminum-copper alloy, 0.4 part of aluminum-erbium alloy, 0.0015 part of refiner Al-5Ti-B, 0.06 part of modifier Sr and 0.5 part of refiner hexachloroethane;
(2) smelting: adding pure aluminum into a coreless medium-frequency induction furnace, raising the furnace temperature to 740 ℃, starting ultrasonic vibration for 20s when the temperature reaches 720 ℃, after the metal is completely melted, adding an intermediate alloy, a modifier and a refiner by a bell jar pressing method, carrying out electromagnetic stirring during the process, and then starting refining and slagging off;
(3) casting the prepared alloy liquid into ingots, and then carrying out multidirectional forging, homogenization treatment, rolling, stress relief annealing, low-temperature continuous ECAP, precipitation strengthening, drawing and twisting on the alloy ingots.
The invention has the advantages that: a water-cooled metal mold or a copper mold is adopted to ensure that the prepared ultrafine grain material is obtained; the low-temperature ECAP technology is adopted, so that the service life of the material can be prevented from being reduced due to the growth of crystal grains in the deformation process; the casting of ingots and then the multidirectional forging are adopted, so that the casting defect of the structure can be eliminated, and the uniformity of the material structure is greatly improved; the aluminum alloy conductor has the characteristics of light weight, good conductivity and the like, but the traditional aluminum alloy conductor has poor heat resistance and cannot meet various requirements of various industries, so the key point of the invention is as follows: preparing ultra-fine crystals; the material prepared by the method has greatly improved heat resistance, fatigue resistance and fatigue life; the preparation of the alloy comprehensively considers the grain refinement in the melting and solidification processes and the grain refinement in the low-temperature processing process, thereby ensuring that the material has fine grain grade (nano grade or submicron grade, and other people do not use the method to prepare the ultra-fine grain heat-resistant aluminum alloy wire), refining the grains and greatly improving the comprehensive performance of the material; the crystal grain can be thinned to be between 100nm and 10 mu m by using the method, the size of the crystal grain can be ensured to be less than 5 mu m after low-temperature ECAP treatment, and the conductivity is basically not influenced; by adopting strengthening means such as solid solution strengthening, deformation strengthening, fine grain strengthening, precipitation strengthening and the like, the material is ensured to have higher strength and heat resistance, so that the material has the performance which is not possessed by common materials; due to the fact that the A/C path is carried out for low-temperature continuous ECAP, directional twinning is generated in the aluminum alloy lead, the strength and the conductivity are improved, meanwhile, the thermal stability of an aluminum alloy structure is improved, and the aluminum alloy lead has excellent oxidation resistance and fatigue resistance. The invention has good application and development prospect.
Detailed Description
The invention relates to a preparation method of a superfine-grain high-strength-toughness heat-resistant aluminum alloy wire, which comprises the following steps:
(1) preparing materials: the composition comprises the following components in parts by weight: 100 parts of industrial pure aluminum, 0.7 part of aluminum-zirconium alloy, 0.4 part of aluminum-copper alloy, 0.4 part of aluminum-erbium alloy, 0.0015 part of refiner Al-5Ti-B, 0.06 part of modifier Sr and 0.5 part of refiner hexachloroethane;
(2) smelting: adding pure aluminum into a coreless medium-frequency induction furnace, raising the furnace temperature to 740 ℃, starting ultrasonic vibration for 20s when the temperature reaches 720 ℃, after the metal is completely melted, adding an intermediate alloy, a modifier and a refiner by a bell jar pressing method, carrying out electromagnetic stirring during the process, and then starting refining and slagging off;
(3) casting the prepared alloy liquid into ingots, and then carrying out multidirectional forging, homogenization treatment, rolling, stress relief annealing, low-temperature continuous ECAP, precipitation strengthening, drawing and twisting on the alloy ingots.
The following preparation is made in advance in the links of alloy smelting, pouring, homogenization treatment, low-temperature continuous ECAP and the like:
under the protection of inert gas, smelting high-purity aluminum and an intermediate alloy, adding a refining agent and a refiner, and preparing an alloy solution; preparing materials: adopts more than 99.99 percent of high-purity aluminum, aluminum erbium intermediate alloy, aluminum magnesium intermediate alloy, aluminum copper intermediate alloy and aluminum silicon intermediate alloy which are coated by pure aluminum foil. And a refiner, a modifier and a refining agent coated by the pure aluminum foil. Preparing a coating: 10% of water glass, 10% of ZnO and 80% of water. Pouring water glass into 90% hot water, stirring to mix fully, then adding ZnO solid powder and stirring to be uniform; and uniformly coating the inner wall of the copper mold, the slag removing spoon, the stirring rod and the refining tool with paint, and carrying out rust removal treatment on the surface before the paint.
The method comprises the following specific steps: adding a master alloy: simultaneously adding an aluminum-magnesium intermediate alloy, an aluminum-silicon intermediate alloy, an aluminum-zirconium intermediate alloy and an aluminum-erbium intermediate alloy by using a bell jar method;
modification, refinement and refining treatment: after the intermediate alloy is completely melted, Al-5Ti-B refiner and Sr alterant are added by a bell jar method, and hexachloroethane is added for refining and slagging off.
The method comprises the following specific steps: pouring: when the temperature is slowly cooled to 720 ℃ along with the furnace, the molten metal is poured into a water-cooling copper mold or a steel mold for rapid solidification, and in the process, secondary ultrasonic vibration is applied to the molten aluminum to refine crystal grains and prevent the crystal grains from growing.
The method comprises the following specific steps: multidirectional forging: and (4) carrying out multidirectional forging on the cast ingot, and crushing coarse columnar crystals and isometric crystals to ensure that the microstructure of the material is uniformly distributed.
The method comprises the following specific steps: homogenizing: after solidification, carrying out solid solution treatment on the cast ingot at 500-590 ℃, and keeping the temperature for 8 h; improve the chemical composition and the structure uniformity of the cast ingot, enable the structure to reach or approach the equilibrium state and improve the plasticity.
The method comprises the following specific steps: rolling: rolling into a small-diameter rod material with the diameter of about phi 10 at room temperature;
stress relief annealing: keeping the temperature of the vacuum furnace at 160 +/-10 ℃ for 4.5 +/-0.5 h, and cooling in air.
The method comprises the following specific steps: low temperature treatment and continuous low temperature ECAP: putting the rolled rod material into an ECAP mould, and carrying out continuous low-temperature ECAP-A path (in the original direction after extrusion) for 2-4 times by using ｃA dry ice cooling mould;
from the second pass, stress relief annealing is needed before each extrusion, the temperature of the vacuum furnace is 160 +/-10 ℃, the temperature is kept for 4.5 +/-0.5 h, and air cooling is carried out; then the low-temperature ECAP-A path deformation is carried out.
The method comprises the following specific steps: precipitation strengthening: and (4) keeping the temperature of the vacuum furnace at 180 +/-5 ℃ for 5-8 hours, and cooling in air.
The method comprises the following specific steps: drawing: and continuously drawing the alloy subjected to stress relief annealing into an alloy wire with the required diameter by utilizing the ductility of the aluminum alloy.
The method comprises the following specific steps: stranding: and twisting the drawn alloy wire into an alloy wire according to the requirement.
The invention is further developed with the following more specific examples.
The first embodiment is as follows: the invention relates to a preparation method of a superfine-grain high-strength-toughness heat-resistant aluminum alloy wire, which comprises the following steps:
step (1) preparing materials: industrial pure aluminum (99.99%), AI-Er (Er: 12.61% Si:0.013% Fe:0.051% Ca: 0.0048%) master alloy, AI-Cu (Cu: 51.96% Si:0.013% Fe:0.018% Ca: 0.0025%) master alloy, Al-Zr (Zr: 10.60%) master alloy, and Al-5Ti-B refiner Sr alterant and hexachloroethane refiner.
And (2) preheating the furnace charge in an oven at 210-220 ℃ for 30min, fully drying, smelting in a white corundum crucible at 750 ℃, stirring, slagging off, measuring the temperature, adding an intermediate alloy at 740 ℃, stirring for 30s, and shaking for 30 s. Keeping the temperature for 3min, adding a refining agent after temperature measurement, shaking for 30s, slagging off, and opening the heat preservation box. Pouring into a copper mould when the temperature is reduced to 725 ℃. The prepared zinc oxide coating is evenly coated on a die cavity and a riser end, the zinc oxide coating is taken out and assembled for casting two minutes before casting, hexachloroethane is also wrapped in aluminum foil and placed in an air drying box for drying, and the temperature of the drying box is 2 ℃. Adding pure aluminum into a corundum crucible of a coreless medium-frequency induction furnace, placing other intermediate alloy and furnace burden into a bell jar, heating the furnace to 740 ℃, starting ultrasonic vibration for 20s when the temperature reaches 720 ℃, and adding the intermediate alloy in specified parts by a bell jar pressing method after the metal is completely melted.
And (3) performing electromagnetic stirring, namely adding the intermediate alloy into the completely molten pure aluminum liquid by using a bell jar pressing method, and then performing electromagnetic stirring in a medium-frequency induction furnace for 3-5 minutes to fully mix the melt.
The electromagnetic stirring technology is used for replacing manual stirring, and not only is the uniformity of chemical components of a melt improved and the quality of an aluminum alloy greatly improved, but also the oxidizing slag can be directionally moved to facilitate slag skimming by one of important technical means for improving the product quality, reducing the consumption of aluminum resources, saving energy and improving the product quality of aluminum processing materials.
Too high a surface temperature of the bath without stirring results in a higher oxidation rate; during manual stirring, strong turbulence is generated on the surface of the molten pool, so that a large amount of aluminum molten drops are involved in the slag layer, and the temperature in the molten pool is more stable due to electromagnetic stirring.
Step (4), refiner and modifier: after the master alloy is completely melted, the furnace temperature is raised to 740-750 ℃, Al-5Ti-B refiner and Sr alterant in specified parts are added, then the melt is electromagnetically stirred for 5min, and the furnace temperature is stably controlled at 730 ℃ after the stirring is finished. And then refining and purifying the melt by using a hexachloroethane refining agent. The refining time is based on the completion of the consumption of the refining agent, various impurities and gases in the aluminum alloy are removed, the purity of the aluminum liquid is further improved, the uniformity of the refining effect is improved, the generation of harmful phases is avoided, and the finally obtained material with uniform grain size and good mechanical property is obtained.
Step (5) casting: and regulating the furnace temperature to 720 ℃, and pouring the alloy liquid into a round ingot blank in a copper mold.
The prepared coating is sprayed, so that the impact of a melt on a copper mold in the pouring process can be weakened by the coating, the mold is protected, the damage of the mold is avoided, the casting precision can be improved, the surface of the casting is smooth and clean, and the casting can be conveniently separated from the casting mold.
Immersing an ultrasonic head into a melt for about 15mm in the process of aluminum liquid solidification, and carrying out isothermal ultrasonic vibration for about 20s at 720 ℃ to refine the primary crystal phase; and then pouring the aluminum liquid into a copper mold, and applying secondary ultrasonic vibration to the aluminum liquid at a eutectoid temperature stage to fully refine crystal grains. The smelting temperature is controlled not to exceed 760 ℃, when the smelting temperature exceeds 770 ℃, the oxidation of the alloy is serious, the hydrogen absorption and slag inclusion in the smelting process are increased, the crystal grains are coarse in the casting and solidification process, and the mechanical property is reduced.
Step (6) multidirectional forging: and (3) performing multidirectional forging on the cast ingot, crushing columnar crystals formed in the cast ingot at an early stage, and homogenizing the material structure.
Step (7) solution treatment: homogenizing the cast ingot at 560-590 ℃, wherein the homogenizing time is 6-8h (the homogenizing time can be properly shortened along with the increase of the temperature).
Step (8) rolling: and continuously rolling the alloy ingot subjected to multidirectional forging into a rod or wire with the diameter of 10 +/-2 mm.
Step (9) stress relief annealing: and (3) preserving the heat of the rolled alloy at 150 ℃ for 4h for stress relief annealing.
Step (10) continuous equal channel angular extrusion (ECAP-conform): according to the requirements of the aluminum stranded wire on the size and diameter specifications, a die with a groove with the corresponding wire diameter size is arranged on continuous ECAP equipment, and MoS is uniformly coated in a die channel before extrusion2A lubricant; the rolled aluminum alloy rod continuously passes through dry ice, the material is cooled at low temperature (-78.5 ℃) and is extruded at low temperature and continuous equal channel corner. Adopting an ECAP mould with a channel angle of 105 degrees and adopting an A path, firstly soaking a rolled rod material in dry ice for 3 minutes, and uniformly coating MoS on the surfaces of a mould channel and a cooling rod material of a continuous ECAP extruder2And (3) a lubricant. Wrapping dry ice around the die channel before and during extrusion to prevent the die temperature from rising during extrusion; then continuous ECAP extrusion is carried out at a medium-low speed of 6-10mm/s, the diameter of the extruded wire is changed into a size range (6-10 mm) through a necking at an outlet of a die channel, and the wire is enabled to form an ultrafine fiber structure in the extrusion direction.
Step (11), precipitation strengthening: the artificial aging (precipitation strengthening) is carried out at the aging temperature of 130 ℃ for 4-8 h.
Step (12) drawing: and adjusting the air pressure and the wire moving speed of the drawing machine, continuously drawing the wire annealed by the ECAP extruder on the drawing machine, and enabling the diameter of the wire to meet the dimension specification of a single bare wire of a stranded wire to finally obtain the aluminum alloy monofilament.
Step (13), stranding: twisting the obtained aluminum alloy monofilaments into a conductor according to requirements.
Example two:
the difference between the embodiment and the first embodiment is that the mold angle adopted in the step (10) is 120 °.
Example three:
the difference between the present embodiment and the first embodiment is that the mold angle adopted in the step (10) is 135 °.
Example four:
the present embodiment is different from the first embodiment in that the extrusion path adopted in the step (10) is C.
Example five:
this example differs from example one in that the ageing temperature used in step (11) is 150 ℃.
Example six:
this example differs from example one in that the ageing temperature used in step (11) is 170 ℃.
Example seven:
the present embodiment is different from the first embodiment in that the casting mold used in the step (5) is a water-cooled steel mold.
Claims (10)
1. A preparation method of a superfine-grain high-strength-toughness heat-resistant aluminum alloy wire is characterized by comprising the following steps:
(1) preparing materials: the composition comprises the following components in parts by weight: 100 parts of industrial pure aluminum, 0.7 part of aluminum-zirconium alloy, 0.4 part of aluminum-copper alloy, 0.4 part of aluminum-erbium alloy, 0.0015 part of refiner Al-5Ti-B, 0.06 part of modifier Sr and 0.5 part of refiner hexachloroethane;
(2) smelting: adding pure aluminum into a coreless medium-frequency induction furnace, raising the furnace temperature to 740 ℃, starting ultrasonic vibration for 20s when the temperature reaches 720 ℃, after the metal is completely melted, adding an intermediate alloy, a modifier and a refiner by a bell jar pressing method, carrying out electromagnetic stirring during the process, and then starting refining and slagging off;
(3) casting the prepared alloy liquid into ingots, and then carrying out multidirectional forging, homogenization treatment, rolling, stress relief annealing, low-temperature continuous ECAP, precipitation strengthening, drawing and twisting on the alloy ingots.
2. The preparation method of the ultra-fine grained high-toughness heat-resistant aluminum alloy wire according to claim 1, which is characterized by comprising the following steps: adding a master alloy: simultaneously adding an aluminum-magnesium intermediate alloy, an aluminum-silicon intermediate alloy, an aluminum-zirconium intermediate alloy and an aluminum-erbium intermediate alloy by using a bell jar method;
modification, refinement and refining treatment: after the intermediate alloy is completely melted, Al-5Ti-B refiner and Sr alterant are added by a bell jar method, and hexachloroethane is added for refining and slagging off.
3. The preparation method of the ultra-fine grained high-toughness heat-resistant aluminum alloy wire according to claim 1, which is characterized by comprising the following steps:
pouring: when the temperature is slowly cooled to 720 ℃ along with the furnace, the molten metal is poured into a water-cooling copper mold or a steel mold for rapid solidification, and in the process, secondary ultrasonic vibration is applied to the molten aluminum to refine crystal grains and prevent the crystal grains from growing.
4. The preparation method of the ultra-fine grained high-toughness heat-resistant aluminum alloy wire according to claim 1, which is characterized by comprising the following steps:
multidirectional forging: and (4) carrying out multidirectional forging on the cast ingot, and crushing coarse columnar crystals and isometric crystals to ensure that the microstructure of the material is uniformly distributed.
5. The preparation method of the ultra-fine grained high-toughness heat-resistant aluminum alloy wire according to claim 1, which is characterized by comprising the following steps:
homogenizing: after solidification, carrying out solid solution treatment on the cast ingot at 500-590 ℃, and keeping the temperature for 8 h; improve the chemical composition and the structure uniformity of the cast ingot, enable the structure to reach or approach the equilibrium state and improve the plasticity.
6. The preparation method of the ultra-fine grained high-toughness heat-resistant aluminum alloy wire according to claim 1, which is characterized by comprising the following steps:
rolling: rolling into a small-diameter rod material with the diameter of about phi 10 at room temperature;
stress relief annealing: keeping the temperature of the vacuum furnace at 160 +/-10 ℃ for 4.5 +/-0.5 h, and cooling in air.
7. The preparation method of the ultra-fine grained high-toughness heat-resistant aluminum alloy wire according to claim 1, which is characterized by comprising the following steps:
low temperature treatment and continuous low temperature ECAP: putting the rolled rod material into an ECAP mould, and carrying out low-temperature continuous ECAP-A path (in the original direction after extrusion) continuous extrusion for 2-4 times by using ｃA dry ice cooling mould;
from the second pass, stress relief annealing is needed before each extrusion, the temperature of the vacuum furnace is 160 +/-10 ℃, the temperature is kept for 4.5 +/-0.5 h, and air cooling is carried out;
then the low-temperature ECAP-A path deformation is carried out.
8. The preparation method of the ultra-fine grained high-toughness heat-resistant aluminum alloy wire according to claim 1, which is characterized by comprising the following steps:
precipitation strengthening: and (4) keeping the temperature of the vacuum furnace at 180 +/-5 ℃ for 5-8 hours, and cooling in air.
9. The preparation method of the ultra-fine grained high-toughness heat-resistant aluminum alloy wire according to claim 1, which is characterized by comprising the following steps:
drawing: and continuously drawing the alloy subjected to stress relief annealing into an alloy wire with the required diameter by utilizing the ductility of the aluminum alloy.
10. The preparation method of the ultra-fine grained high-toughness heat-resistant aluminum alloy wire according to claim 1, which is characterized by comprising the following steps:
stranding: and twisting the drawn alloy wire into an alloy wire according to the requirement.
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| CN113385549A (en) * | 2021-07-07 | 2021-09-14 | 兰州理工大学 | Composite processing method of high-strength high-conductivity pure copper wire |
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| CN115011847A (en) * | 2022-06-20 | 2022-09-06 | 江苏凯特汽车部件有限公司 | Preparation technology of graphene rare earth composite reinforced Al-Si-Cu-Mg material |
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| CN113684388A (en) * | 2021-08-27 | 2021-11-23 | 江苏中天科技股份有限公司 | High-conductivity soft aluminum monofilament and preparation method thereof |
| CN113684388B (en) * | 2021-08-27 | 2022-04-26 | 江苏中天科技股份有限公司 | High-conductivity soft aluminum monofilament and preparation method thereof |
| CN115011847A (en) * | 2022-06-20 | 2022-09-06 | 江苏凯特汽车部件有限公司 | Preparation technology of graphene rare earth composite reinforced Al-Si-Cu-Mg material |
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