CN108048707B - Preparation method of corrosion-resistant aluminum alloy material containing gadolinium and yttrium - Google Patents
Preparation method of corrosion-resistant aluminum alloy material containing gadolinium and yttrium Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 119
- 238000005260 corrosion Methods 0.000 title claims abstract description 54
- 230000007797 corrosion Effects 0.000 title claims abstract description 53
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 51
- 229910052688 Gadolinium Inorganic materials 0.000 title claims abstract description 18
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 14
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 97
- 238000000034 method Methods 0.000 claims abstract description 45
- 238000004512 die casting Methods 0.000 claims abstract description 31
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000007670 refining Methods 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 11
- 239000010949 copper Substances 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 74
- 239000000155 melt Substances 0.000 claims description 48
- 238000007792 addition Methods 0.000 claims description 43
- 229910052786 argon Inorganic materials 0.000 claims description 37
- 238000010438 heat treatment Methods 0.000 claims description 32
- 239000011265 semifinished product Substances 0.000 claims description 31
- 238000002347 injection Methods 0.000 claims description 25
- 239000007924 injection Substances 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 25
- 238000001816 cooling Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 22
- 238000004321 preservation Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 18
- 230000032683 aging Effects 0.000 claims description 16
- 239000004576 sand Substances 0.000 claims description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000005070 sampling Methods 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 5
- 230000002431 foraging effect Effects 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000000047 product Substances 0.000 claims 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 14
- 150000002910 rare earth metals Chemical class 0.000 abstract description 14
- 229910018594 Si-Cu Inorganic materials 0.000 abstract description 11
- 229910008465 Si—Cu Inorganic materials 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 4
- 239000013535 sea water Substances 0.000 abstract description 4
- 229910018191 Al—Fe—Si Inorganic materials 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 239000010410 layer Substances 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011241 protective layer Substances 0.000 abstract description 2
- 239000006104 solid solution Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 11
- 238000003723 Smelting Methods 0.000 description 7
- 229910000851 Alloy steel Inorganic materials 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 229910000946 Y alloy Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 229910000748 Gd alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- 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
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- 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
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- 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
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- 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
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- 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
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
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- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
A preparation method of a corrosion-resistant aluminum alloy material containing gadolinium and yttrium comprises the following steps of: 9.6-12 wt.% of silicon, 1.5-3.5 wt.% of copper, 0.4-0.6 wt.% of gadolinium, 0.4-0.6 wt.% of yttrium, and the balance of aluminum and inevitable impurities. Controlling the content of different elements in the alloy, refining by rare earth gadolinium, and then carrying out die-casting molding. The aluminum alloy material prepared by the method has high surface smoothness, a more compact surface aluminum oxide protective layer and excellent seawater corrosion resistance, and can meet the application in marine environment; can lead rare earth Gd to be Al in the alloy2A layer of rare earth coating film is formed on the surface of intermetallic compounds such as Cu, Al-Fe-Si and the like, so that the flow of corrosion electrons is hindered; the solid solubility of the die-casting Al-Si-Cu alloy can be improved, and the influence of galvanic corrosion is further reduced; the operation is safe and simple, the requirement on equipment is low, and the manufacturing cost is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of metal material manufacturing, and particularly relates to a corrosion-resistant aluminum alloy.
Background
The Al-Si-Cu alloy has good casting performance, higher air tightness, good cutting processing performance and weldability, and higher strength after heat treatment and strengthening. Due to Al in the Al-Si-Cu alloy2The corrosion potential of Cu and Al-Fe-Si intermetallic compounds in seawater is higher than that of α -Al matrix, so that Al-Si-Cu alloy can be locally corroded in seawater.
So far, the refining methods for Al-Si-Cu alloy mainly include: adding rare earth or alkaline earth elements, and performing electromagnetic stirring and ultrasonic treatment. However, in the method, the rare earth adding refining method is simple in technical operation, low in equipment requirement and beneficial to large-scale production, and the microstructure and mechanical properties of the alloy are far superior to those of a matrix due to the rare earth refining method. In addition, the technology for manufacturing the aluminum alloy material by pressure casting is one of the most advanced metal forming methods, is an effective way for realizing less cutting scraps and no cutting scraps, has wide application and is developed quickly. And the die casting material can realize high surface finish and internal grain refinement. The corrosion rate can be reduced to some extent.
Solution aging is also commonly used to improve the properties of aluminum alloys as a low cost method of improving the toughness and corrosion resistance. In addition, the invention utilizes a two-stage solution treatment mode to lead the material to undergo two stages of low temperature and high temperature. The low melting point phase is dissolved first during low-temperature solid solution, and overburning and melting at high temperature are prevented. And the second phase particles are dissolved during high-temperature solid solution, so that the supersaturation degree of the alloy is improved.
In published patent No. CN104711460B, the name is: a titanium-containing corrosion-resistant aluminum alloy and a treatment process thereof. The smelting sequence and the smelting time of part of different alloy elements are not considered in the smelting process, and the internal stress of the alloy elements is eliminated without a heat treatment process after refining.
In published patent No. CN103966483B, the name is: an anti-corrosion aluminum alloy plate for automobiles. Firstly, smelting and atomizing to prepare alloy micron powder, then smelting the alloy powder again, adding a refining agent for refining, and finally carrying out multi-stage low-temperature cold treatment to obtain the corrosion-resistant aluminum alloy plate for the automobile. The process is novel, but compared with the heat treatment, the multi-stage low-temperature cold treatment has relatively simple heat treatment procedures and is convenient for actual production.
In published patent No. CN105112738B, the name is: a preparation process of high-strength corrosion-resistant aluminum alloy and the high-strength corrosion-resistant aluminum alloy. The high-strength corrosion-resistant aluminum alloy is obtained by combining high-temperature refining and solution treatment. However, the time for pure high-temperature refining and solution treatment is long, and the refining and solution treatment time is greatly shortened if a small amount of refining agent is added in the refining process.
In published patent No. CN104962786B, the name is: a corrosion-resistant aluminum alloy section. And carrying out heat treatment on the horizontally cast section by utilizing secondary aging treatment to obtain the corrosion-resistant aluminum alloy section. The method is not subjected to solid solution treatment before secondary aging to obtain a uniform supersaturated solid solution, and is directly subjected to artificial aging, so that precipitation of a strengthening phase during later aging and elimination of internal stress during early thermal processing are not facilitated.
Therefore, in summary, there is still no economical and effective solution for the preparation and forming technology of the corrosion-resistant die-casting aluminum alloy material. And the influence of rare earth Gd as an alloying element on the enhancement of the corrosion resistance of the Al-Si-Cu alloy is not reported, so that the method has great research value.
Disclosure of Invention
The invention aims to provide a preparation method of a corrosion-resistant die-casting aluminum alloy containing gadolinium and yttrium.
The invention is realized by the following technical scheme.
A preparation method of a corrosion-resistant aluminum alloy material containing gadolinium and yttrium is characterized by comprising the following steps.
(1) The composite material comprises the following elements in percentage by mass: 9.6-12 wt.% of silicon, 1.5-3.5 wt.% of copper, 0.4-0.6 wt.% of gadolinium and 0.4-0.6 wt.% of yttrium, with the balance being aluminum and inevitable impurities; the total of said unavoidable impurities is present in the alloy in an amount not exceeding 0.3wt.%, and the iron content of said unavoidable impurities is present in the alloy in an amount not exceeding 0.1 wt.%.
(2) Melting a certain mass of pure aluminum ingot in a corundum crucible with the melting temperature of 730-750 ℃, and preserving heat for 5-10 minutes.
(3) Raising the temperature of the furnace in the step (2) to 830-850 ℃, then averagely dividing the pre-dried Al-10Si alloy into a plurality of equal parts, adding the equal parts into the heated melt, wherein the adding amount of the Al-10Si alloy is 2.0-3.5 wt.% of the total mass of the melt each time; stirring by adopting a double-blade stirrer after each addition, standing and preserving heat for 5-10 minutes after all the additions, and introducing argon for protection in the process.
(4) Equally dividing the pre-dried Al-10Cu alloy into a plurality of equal parts, and adding the equal parts into the melt in the step (3), wherein the adding amount of the Al-10Cu alloy in each time is 0.15-0.3 wt.% of the total mass of the melt; stirring by adopting a double-blade stirrer after each addition, standing and preserving heat for 5-10 minutes after all the additions, and introducing argon for protection in the process.
(5) And (4) refining, namely equally dividing the pre-dried Al-10Gd alloy into a plurality of equal parts, and adding the equal parts into the melt in the step (4), wherein the amount of the Al-10Gd alloy added in each time is 0.1-0.3 wt% of the total mass of the melt. And carrying out ultrasonic treatment after each addition, wherein the ultrasonic power is 650-700W, the ultrasonic frequency is 25000-30000 Hz, the ultrasonic time is in direct proportion to the addition amount of the Al-10Gd alloy, and the ultrasonic time is increased by 2-3 min when the addition amount of the Al-10Gd alloy is increased by 0.1 wt.%. And standing and preserving the heat for 20-25 minutes after all the components are added. Argon is introduced for protection in the process; and after stirring and standing are finished, slagging off the obtained mixed melt, sampling and analyzing the mixed melt after slagging off, and reducing the temperature of the melt with qualified components to 680-710 ℃ for heat preservation for later use.
(6) And (3) equally dividing the pre-dried Al-10Y alloy into a plurality of equal parts, adding the equal parts into the melt in the step (5), wherein the amount of the Al-10Y alloy added in each time is 0.1-0.3 wt% of the total mass of the melt. And carrying out ultrasonic treatment after each addition, wherein the ultrasonic power is 700-735W, the ultrasonic frequency is 27000-32500 Hz, the ultrasonic time is in direct proportion to the addition of the Al-10Y alloy, and the ultrasonic time is increased by 2-3 min when the addition of the Al-10Y alloy is increased by 0.1 wt.%. And standing and preserving the heat for 20-30 minutes after all the components are added. Argon is introduced for protection in the process; and after stirring and standing are finished, slagging off the obtained mixed melt, sampling and analyzing the mixed melt after slagging off, and reducing the temperature of the melt with qualified components to 680-710 ℃ for heat preservation for later use.
(7) And (4) pouring the melt with qualified components obtained in the step (6) into a pouring gate of a die casting machine, and die-casting the melt into a columnar aluminum alloy material. The die casting process is set as follows: the casting temperature is 680-710 ℃, the thickness of the material handle is 25mm, and the mold temperature is 150-170 ℃. The injection force was 330kN and the hammer diameter was 60 mm. The injection pressure is 116MPa, the injection time is 3S, the cooling time is 2S, and the mold remaining time is 10S. The die handle action stroke position in the die-casting process is as follows: the slow injection starting position is 80mm, the fast injection starting position is 270mm, the pressurization position is 280mm, and the tracking position is 350 mm.
(8) And (3) placing the aluminum alloy material obtained in the step (7) into a resistance furnace for primary solution treatment, wherein the temperature of the solution treatment is 430 +/-3 ℃, the heat preservation time is 2-3 hours, and then, quickly placing the aluminum alloy material into water at the temperature of 60-70 ℃ for cooling.
(9) And (3) placing the material obtained in the step (8) in a resistance furnace for secondary solution treatment, wherein the temperature of the solution treatment is 470 +/-3 ℃, the heat preservation time is 1-2 hours, and then, quickly placing the material in water at the temperature of 60-70 ℃ for cooling.
(10) And (4) placing the material obtained in the step (9) at a temperature of 125 +/-3 ℃ for aging treatment, wherein the aging time is 5-6 hours, and then performing air cooling to obtain the gadolinium and yttrium-containing corrosion-resistant die-casting aluminum alloy.
Further, the solution treatment environment in step (8) of the present invention is: coating the corrosion-resistant aluminum alloy semi-finished product by using granular round sand to ensure uniform heating; secondly, the solid solution temperature is 430 +/-3 ℃, and the heating rate is 20-35 ℃/min; the heat preservation time is 2.5-3.5 hours, and the alloy semi-finished product is placed in a furnace from room temperature.
Further, the solution treatment environment in step (9) of the present invention is: coating the corrosion-resistant aluminum alloy semi-finished product by using granular round sand to ensure uniform heating; secondly, the solid solution temperature is 470 +/-3 ℃, and the heating rate is 20-35 ℃/min; the heat preservation time is 1.5-2.5 hours, and the alloy semi-finished product is placed in a furnace from room temperature.
Further, the aging treatment environment in step (10) of the present invention is: coating the corrosion-resistant aluminum alloy semi-finished product subjected to solution treatment by using granular round sand, and ensuring uniform heating; secondly, the solid solution temperature is 125 +/-3 ℃, and the heating rate is 15-25 ℃/min; and (5) keeping the temperature for 5-6 hours, and placing the alloy semi-finished product in a furnace from room temperature.
The invention utilizes rare earth Gd + Y refining technology to weaken Al in the alloy2The galvanic corrosion reaction between intermetallic compounds such as Cu and Al-Fe-Si and the like and the aluminum matrix does not affect the excellent properties inherent in the Al-Si-Cu alloy. And secondly, performing die-casting molding by using Al-Si-Cu alloy melt refined by rare earth Gd + Y to obtain the aluminum alloy material with high surface smoothness and compact structure, wherein the smooth surface of the material and the compact surface alumina structure can also improve the corrosion resistance of the alloy to a certain extent. Compared with single rare earth, the mixed rare earth can greatly improve the solid solubility of the die-casting Al-Si-Cu alloy. Therefore, the subsequent targeted solution aging treatment can fully dissolve the inactive elements such as Cu, Fe and the like and the generated mixed rare earth phase with high thermal stability, so that the microstructure of the Al-Si-Cu-Gd-Y alloy forms a phenomenon of 'large anode-small cathode', the galvanic corrosion influence is further reduced, and the corrosion resistance of the Al-Si-Cu-Gd-Y alloy is greatly improved. The result shows that the corrosion resistance of the alloy of the embodiment of the invention is improved by 1.5 to 3 times compared with the corrosion resistance of the common Al-Si-Cu system.
The invention has the following uniqueness: (1) the aluminum alloy material prepared by the method has high surface smoothness, a more compact surface aluminum oxide protective layer and excellent seawater corrosion resistance, and can meet the application in marine environment; (2) the invention can lead rare earth Gd to be Al in the alloy2Intermetallic compound of Cu and Al-Fe-SiA layer of rare earth coating film is formed on the surface of the compound to block the flow of corrosion electrons; (3) the invention can improve the solid solubility of the die-casting Al-Si-Cu alloy, so that the microstructure of the Al-Si-Cu-Gd alloy forms a phenomenon of 'large anode-small cathode', and the influence of galvanic corrosion is further reduced; (4) the invention has safe and simple operation, low requirement on equipment and greatly reduced manufacturing cost.
Detailed Description
The invention will be further illustrated by the following examples.
Example 1.
(1) According to the proportion of 9.6wt.% of silicon, 1.5wt.% of copper, 0.4wt.% of gadolinium and 0.4wt.% of yttrium and the balance of aluminum, industrial pure aluminum ingots, Al-10Si alloys, Al-10Cu alloys, Al-10Gd alloys and Al-10Y alloys are respectively put into a vacuum drying box, the drying temperature is 70 ℃, and the drying time is 60 minutes.
(2) Placing a corundum crucible in a tubular furnace protected by high-purity argon atmosphere, adding a pure aluminum ingot, melting at 740 ℃, and keeping the temperature for 7 minutes.
(3) And (3) raising the furnace temperature in the step (2) to 835 ℃, and then averagely dividing the pre-dried Al-10Si alloy obtained in the step (1) into a plurality of equal parts to be added into the heated melt, wherein the amount of the Al-10Si alloy added in each time is 2.5wt.% of the total mass of the melt. After each addition, a high-temperature-resistant alloy steel double-blade stirrer is adopted to stir for 1 minute at the speed of 30 revolutions per minute, and after all the additions, the mixture is kept stand and kept warm for 6 minutes. Argon is introduced for protection in the process, the flow of the argon is 20L/min, and the pressure of the argon is 0.45 MPa.
(4) And (3) equally dividing the pre-dried Al-10Cu alloy into a plurality of equal parts, adding the equal parts into the melt in the step (3), wherein the adding amount of the Al-10Cu alloy in each time is 1.5wt.% of the total mass of the melt. After each addition, a high-temperature-resistant alloy steel double-blade stirrer is adopted to stir for 1 minute at the speed of 30 revolutions per minute, and after all the additions, the mixture is kept stand and kept warm for 6 minutes. Argon is introduced for protection in the process, the flow of the argon is 20L/min, and the pressure of the argon is 0.45 MPa.
(5) And (3) equally dividing the pre-dried Al-10Gd alloy into a plurality of equal parts, and adding the equal parts into the melt in the step (4), wherein the amount of the Al-10Gd alloy added in each time is 0.1 wt% of the total mass of the melt. Ultrasonic treatment is carried out after each addition, the ultrasonic power is 650W, the ultrasonic frequency is 25000Hz, and the ultrasonic time is 3 min. After all the addition, the mixture was kept still for 21 minutes. Argon is introduced for protection in the process, the flow of the argon is 20L/min, and the pressure of the argon is 0.45 MPa.
(6) And (3) equally dividing the pre-dried Al-10Y alloy into a plurality of equal parts, adding the equal parts into the melt in the step (5), wherein the adding amount of the Al-10Y alloy in each time is 0.1wt.% of the total mass of the melt. Ultrasonic treatment is carried out after each addition, the ultrasonic power is 700W, the ultrasonic frequency is 27000Hz, and the ultrasonic time is 3 min. After all the addition, the mixture is kept stand and kept warm for 20 minutes. Argon is introduced for protection in the process.
(7) And (4) slagging off the mixed melt obtained after the stirring and standing in the step (6), sampling and analyzing the slag, and cooling the melt with qualified components to 680 ℃ for heat preservation for later use.
(8) Pouring the melt with qualified components obtained in the step (7) into a pouring gate of a die casting machine, and die-casting into a columnar aluminum alloy material. The die casting process is set as follows: the casting temperature is 680 ℃, the thickness of the material handle is 25mm, and the mold temperature is 150 ℃. The injection force was 330kN and the hammer diameter was 60 mm. The injection pressure is 116MPa, the injection time is 3S, the cooling time is 2S, and the mold remaining time is 10S. The die handle action stroke position in the die-casting process is as follows: the slow injection starting position is 80mm, the fast injection starting position is 270mm, the pressurization position is 280mm, and the tracking position is 350 mm.
(9) Putting the die-casting material obtained in the step (8) into a box-type resistance furnace for primary solution treatment, and coating a corrosion-resistant aluminum alloy semi-finished product by using granular round sand to ensure uniform heating; secondly, the solid solution temperature is 428 ℃, and the heating rate is 22 ℃/min; the heat preservation time is 2 hours, the alloy semi-finished product is placed in a furnace from room temperature, and then is rapidly placed in water with the temperature of 60 ℃ for cooling.
(10) Placing the corrosion-resistant aluminum alloy semi-finished product obtained in the step (9) in a box-type resistance furnace for secondary solution treatment, and coating the corrosion-resistant aluminum alloy semi-finished product with granular round sand to ensure uniform heating; secondly, the solid solution temperature is 468 ℃, and the heating rate is 25 ℃/min; the heat preservation time is 1.7 hours, the alloy semi-finished product is placed in a furnace from room temperature, and then is quickly placed in water with the temperature of 65 ℃ for cooling.
(11) Coating the material obtained in the step (10) by using granular round sand, and placing the coated material into an environment with the aging temperature of 123 ℃ and the heating rate of 17 ℃/min for aging treatment; the heat preservation time is 5 hours, and the alloy semi-finished product is placed in a furnace from room temperature. And after the aging is finished, air cooling to obtain the corrosion-resistant aluminum alloy.
Example 2.
(1) According to the proportion of silicon 10.2wt.%, copper 2.5wt.%, gadolinium 0.5wt.%, yttrium 0.5wt.% and the balance aluminum, industrial pure aluminum ingots, Al-10Si alloys, Al-10Cu alloys, Al-10Gd alloys and Al-10Y alloys are respectively put into a vacuum drying box, the drying temperature is 70 ℃, and the drying time is 60 minutes.
(2) Placing a corundum crucible in a tubular furnace protected by high-purity argon atmosphere, adding pure aluminum ingot, and keeping the temperature for 8 minutes at the smelting temperature of 745 ℃.
(3) And (3) raising the furnace temperature in the step (2) to 840 ℃, and then averagely dividing the pre-dried Al-10Si alloy obtained in the step (1) into a plurality of equal parts to be added into the heated melt, wherein the amount of the Al-10Si alloy added in each time is 3.0wt.% of the total mass of the melt. After each addition, a high-temperature-resistant alloy steel double-blade stirrer is adopted to stir for 1 minute at the speed of 30 revolutions per minute, and after all the additions, the mixture is kept stand and kept warm for 6 minutes. Argon is introduced for protection in the process, the flow of the argon is 20L/min, and the pressure of the argon is 0.45 MPa.
(4) And (3) equally dividing the pre-dried Al-10Cu alloy into a plurality of equal parts, and adding the equal parts into the melt in the step (3), wherein the amount of the Al-10Cu alloy added in each time is 1.7wt.% of the total mass of the melt. After each addition, a high-temperature-resistant alloy steel double-blade stirrer is adopted to stir for 1 minute at the speed of 30 revolutions per minute, and after all the additions, the mixture is kept stand and kept warm for 7 minutes. Argon is introduced for protection in the process, the flow of the argon is 20L/min, and the pressure of the argon is 0.45 MPa.
(5) And (3) equally dividing the pre-dried Al-10Gd alloy into a plurality of equal parts, adding the equal parts into the melt in the step (4), wherein the amount of the Al-10Gd alloy added in each time is 0.2wt.% of the total mass of the melt. Ultrasonic treatment is carried out after each addition, the ultrasonic power is 670W, the ultrasonic frequency is 27000Hz, and the ultrasonic time is 5 min. After all the addition, the mixture was kept stand and kept warm for 23 minutes. Argon is introduced for protection in the process, the flow of the argon is 20L/min, and the pressure of the argon is 0.45 MPa.
(6) And (3) equally dividing the pre-dried Al-10Y alloy into a plurality of equal parts, adding the equal parts into the melt in the step (5), wherein the adding amount of the Al-10Y alloy in each time is 0.2wt.% of the total mass of the melt. Ultrasonic treatment is carried out after each addition, the ultrasonic power is 715W, the ultrasonic frequency is 31000Hz, and the ultrasonic time is 6 min. After all the addition, the mixture is kept stand and kept warm for 25 minutes. Argon is introduced for protection in the process.
(7) And (4) slagging off the mixed melt obtained after the stirring and standing in the step (6), sampling and analyzing the mixed melt after slagging off, and reducing the temperature of the melt with qualified components to 700 ℃ for heat preservation for later use.
(8) Pouring the melt with qualified components obtained in the step (7) into a pouring gate of a die casting machine, and die-casting into a columnar aluminum alloy material. The die casting process is set as follows: the casting temperature is 700 ℃, the thickness of the material handle is 25mm, and the mold temperature is 160 ℃. The injection force was 330kN and the hammer diameter was 60 mm. The injection pressure is 116MPa, the injection time is 3S, the cooling time is 2S, and the mold remaining time is 10S. The die handle action stroke position in the die-casting process is as follows: the slow injection starting position is 80mm, the fast injection starting position is 270mm, the pressurization position is 280mm, and the tracking position is 350 mm.
(9) Placing the corrosion-resistant aluminum alloy semi-finished product containing gadolinium obtained in the step (8) in a box-type resistance furnace for first-stage solution treatment, and coating the corrosion-resistant aluminum alloy semi-finished product with granular round sand to ensure uniform heating; secondly, the solid solution temperature is 430 ℃, and the heating rate is 30 ℃/min; the heat preservation time is 2.5 hours, the alloy semi-finished product is placed in a furnace from room temperature, and then is quickly placed in water with the temperature of 63 ℃ for cooling.
(10) Placing the corrosion-resistant aluminum alloy semi-finished product obtained in the step (9) in a box-type resistance furnace for secondary solution treatment, and coating the corrosion-resistant aluminum alloy semi-finished product with granular round sand to ensure uniform heating; secondly, the solid solution temperature is 470 ℃, and the heating rate is 22 ℃/min; the heat preservation time is 2 hours, the alloy semi-finished product is placed in a furnace from room temperature, and then is quickly placed in water with the temperature of 67 ℃ for cooling.
(11) Coating the material obtained in the step (10) by using granular round sand, and placing the coated material into an environment with the aging temperature of 125 ℃ and the heating rate of 20 ℃/min for aging treatment; the heat preservation time is 5.5 hours, and the alloy semi-finished product is placed in a furnace from room temperature. And after the aging is finished, air cooling to obtain the corrosion-resistant aluminum alloy.
Example 3.
(1) According to the proportion of 12wt.% of silicon, 3.5wt.% of copper, 0.6wt.% of gadolinium and 0.6wt.% of yttrium and the balance of aluminum, industrial pure aluminum ingots, Al-10Si alloy, Al-10Cu alloy, Al-10Gd alloy and Al-10Y alloy are respectively put into a vacuum drying box, the drying temperature is 70 ℃, and the drying time is 60 minutes.
(2) Placing a corundum crucible in a tubular furnace protected by high-purity argon atmosphere, adding a certain mass of pure aluminum ingot, smelting at 750 ℃, and keeping the temperature for 10 minutes.
(3) And (3) raising the furnace temperature in the step (2) to 850 ℃, and then averagely dividing the pre-dried Al-10Si alloy obtained in the step (1) into a plurality of equal parts to be added into the heated melt, wherein the amount of the Al-10Si alloy added in each time is 3.5wt.% of the total mass of the melt. After each addition, a high-temperature-resistant alloy steel double-blade stirrer is adopted to stir for 1 minute at the speed of 30 revolutions per minute, and after all the additions, the mixture is kept stand and kept warm for 10 minutes. Argon is introduced for protection in the process, the flow of the argon is 20L/min, and the pressure of the argon is 0.45 MPa.
(4) And (3) equally dividing the pre-dried Al-10Cu alloy into a plurality of equal parts, adding the equal parts into the melt in the step (3), wherein the adding amount of the Al-10Cu alloy in each time is 1.5wt.% of the total mass of the melt. After each addition, a high-temperature-resistant alloy steel double-blade stirrer is adopted to stir for 1 minute at the speed of 30 revolutions per minute, and after all the additions, the mixture is kept stand and kept warm for 10 minutes. Argon is introduced for protection in the process, the flow of the argon is 20L/min, and the pressure of the argon is 0.45 MPa.
(5) And (3) equally dividing the pre-dried Al-10Gd alloy into a plurality of equal parts, adding the equal parts into the melt in the step (4), wherein the amount of the Al-10Gd alloy added in each time is 0.3 wt% of the total mass of the melt. Ultrasonic treatment is carried out after each addition, the ultrasonic power is 700W, the ultrasonic frequency is 30000Hz, and the ultrasonic time is 9 min. After all the addition, the mixture is kept stand and kept warm for 25 minutes. Argon is introduced for protection in the process, the flow of the argon is 20L/min, and the pressure of the argon is 0.45 MPa.
(6) And (3) equally dividing the pre-dried Al-10Y alloy into a plurality of equal parts, adding the equal parts into the melt in the step (5), wherein the adding amount of the Al-10Y alloy in each time is 0.3wt.% of the total mass of the melt. Ultrasonic treatment is carried out after each addition, the ultrasonic power is 735W, the ultrasonic frequency is 32500Hz, and the ultrasonic time is 9 min. After all the components are added, standing and keeping the temperature for 30 minutes.
(7) And (4) slagging off the mixed melt obtained after the stirring and standing in the step (6), sampling and analyzing the slag, and cooling the melt with qualified components to 710 ℃ for heat preservation for later use.
(8) Pouring the melt with qualified components obtained in the step (7) into a pouring gate of a die casting machine, and die-casting into a columnar aluminum alloy material. The die casting process is set as follows: the casting temperature is 710 ℃, the thickness of the material handle is 25mm, and the mold temperature is 170 ℃. The injection force was 330kN and the hammer diameter was 60 mm. The injection pressure is 116MPa, the injection time is 3S, the cooling time is 2S, and the mold remaining time is 10S. The die handle action stroke position in the die-casting process is as follows: the slow injection starting position is 80mm, the fast injection starting position is 270mm, the pressurization position is 280mm, and the tracking position is 350 mm.
(9) Putting the corrosion-resistant aluminum alloy semi-finished product containing gadolinium obtained in the step (8) into a box-type resistance furnace for solution treatment, and coating the corrosion-resistant aluminum alloy semi-finished product containing gadolinium by using granular round sand to ensure uniform heating; secondly, the solid solution temperature is 433 ℃, and the heating rate is 35 ℃/min; the heat preservation time is 3 hours, the alloy semi-finished product is placed in a furnace from room temperature, and then is rapidly placed in water with the temperature of 70 ℃ for cooling.
(10) Placing the corrosion-resistant aluminum alloy semi-finished product obtained in the step (9) in a box-type resistance furnace for secondary solution treatment, and coating the corrosion-resistant aluminum alloy semi-finished product with granular round sand to ensure uniform heating; secondly, the solid solution temperature is 468 ℃, and the heating rate is 25 ℃/min; the heat preservation time is 2.5 hours, the alloy semi-finished product is placed in a furnace from room temperature, and then is quickly placed in water with the temperature of 70 ℃ for cooling.
(11) Coating the material obtained in the step (10) by using granular round sand, and placing the coated material into an environment with the aging temperature of 128 ℃ and the heating rate of 17 ℃/min for aging treatment; and (4) keeping the temperature for 6 hours, putting the alloy semi-finished product into a furnace from room temperature, and after the aging is finished, air-cooling to obtain the corrosion-resistant aluminum alloy.
Claims (1)
1. A preparation method of a corrosion-resistant aluminum alloy material containing gadolinium and yttrium is characterized by comprising the following steps:
(1) the components by mass percent are as follows: 9.6-12 wt.% of silicon, 1.5-3.5 wt.% of copper, 0.4-0.6 wt.% of gadolinium and 0.4-0.6 wt.% of yttrium, with the balance being aluminum and inevitable impurities; the total of said unavoidable impurities is present in the alloy in an amount not exceeding 0.3wt.%, and the iron of said unavoidable impurities is present in the alloy in an amount not exceeding 0.1 wt.%;
(2) melting a certain mass of pure aluminum ingot in a corundum crucible with the melting temperature of 730-750 ℃, and preserving heat for 5-10 minutes;
(3) raising the temperature of the furnace in the step (2) to 830-850 ℃, then averagely dividing the pre-dried Al-10Si alloy into a plurality of equal parts, and adding the equal parts into the heated melt, wherein the amount of the Al-10Si alloy added each time is 2.0-3.5 wt.% of the total mass of the melt; stirring by adopting a double-blade stirrer after each addition, standing and preserving heat for 5-10 minutes after all the additions, and introducing argon for protection in the process;
(4) equally dividing the pre-dried Al-10Cu alloy into a plurality of equal parts, and adding the equal parts into the melt in the step (3), wherein the amount of the Al-10Cu alloy added each time is 0.15-0.3 wt.% of the total mass of the melt; stirring by adopting a double-blade stirrer after each addition, standing and preserving heat for 5-10 minutes after all the additions, and introducing argon for protection in the process;
(5) refining, namely equally dividing the pre-dried Al-10Gd alloy into a plurality of equal parts, and adding the equal parts into the melt in the step (4), wherein the amount of the Al-10Gd alloy added each time is 0.1-0.3 wt% of the total mass of the melt; carrying out ultrasonic treatment after each addition, wherein the ultrasonic power is 650-700W, the ultrasonic frequency is 25000-30000 Hz, the ultrasonic time is in direct proportion to the addition amount of the Al-10Gd alloy, and the ultrasonic time is increased by 2-3 min when the addition amount of the Al-10Gd alloy is increased by 0.1 wt.%; after all the materials are added, standing and preserving heat for 20-25 minutes; argon is introduced for protection in the process; slagging off the mixed melt obtained after stirring and standing are finished, sampling and analyzing the mixed melt after slagging off, and reducing the temperature of the melt with qualified components to 680-710 ℃ for heat preservation for later use;
(6) equally dividing the pre-dried Al-10Y alloy into a plurality of equal parts, and adding the equal parts into the melt in the step (5), wherein the amount of the Al-10Y alloy added each time is 0.1-0.3 wt.% of the total mass of the melt; carrying out ultrasonic treatment after each addition, wherein the ultrasonic power is 700-735W, the ultrasonic frequency is 27000-32500 Hz, the ultrasonic time is in direct proportion to the addition of the Al-10Y alloy, and the ultrasonic time is increased by 2-3 min when the addition of the Al-10Y alloy is increased by 0.1 wt.%; after all the materials are added, standing and preserving heat for 20-30 minutes; argon is introduced for protection in the process; slagging off the mixed melt obtained after stirring and standing are finished, sampling and analyzing the mixed melt after slagging off, and reducing the temperature of the melt with qualified components to 680-710 ℃ for heat preservation for later use;
(7) pouring the melt with qualified components obtained in the step (6) into a pouring gate of a die casting machine, and performing die casting to obtain a columnar aluminum alloy material; the die casting process is set as follows: the casting temperature is 680-710 ℃, the thickness of the material handle is 25mm, and the mold temperature is 150-170 ℃; the injection force is 330kN, and the diameter of the hammer head is 60 mm; the injection pressure is 116MPa, the injection time is 3S, the cooling time is 2S, and the mold remaining time is 10S; the die handle action stroke position in the die-casting process is as follows: the slow-injection starting position is 80mm, the fast-injection starting position is 270mm, the pressurization position is 280mm, and the tracking position is 350 mm;
(8) placing the aluminum alloy material obtained in the step (7) in a resistance furnace for primary solution treatment, and coating a corrosion-resistant aluminum alloy semi-finished product by using granular round sand to ensure uniform heating; the solution treatment temperature is 430 +/-3 ℃, the heating rate is 20-35 ℃/min, the heat preservation time is 2.5-3 hours, the semi-finished alloy product is placed in a furnace from room temperature, and then is rapidly placed in water at the temperature of 60-70 ℃ for cooling;
(9) placing the material obtained in the step (8) in a resistance furnace for secondary solution treatment, and coating a corrosion-resistant aluminum alloy semi-finished product by using granular round sand to ensure uniform heating; the solution treatment temperature is 470 +/-3 ℃, the heating rate is 20-35 ℃/min, the heat preservation time is 1.5-2 hours, the alloy semi-finished product is placed in a furnace from room temperature, and then is rapidly placed in water at the temperature of 60-70 ℃ for cooling;
(10) placing the material obtained in the step (9) at a temperature of 125 +/-3 ℃ for aging treatment, and coating the corrosion-resistant aluminum alloy semi-finished product subjected to solution treatment by using granular round sand to ensure uniform heating; the aging temperature is 125 +/-3 ℃, the heating rate is 15-25 ℃/min, the aging time is 5-6 hours, the alloy semi-finished product is placed in a furnace from room temperature, and then air cooling is carried out to obtain the gadolinium and yttrium-containing corrosion-resistant die-casting aluminum alloy.
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