CN112921200A - Method for preparing ultrafine grained aluminum alloy by using semi-solid forming technology - Google Patents
Method for preparing ultrafine grained aluminum alloy by using semi-solid forming technology Download PDFInfo
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Abstract
The invention belongs to the technical field of ultra-fine grained aluminum alloy, and particularly relates to a method for preparing ultra-fine grained aluminum alloy by using a semi-solid forming technology. The method comprises the steps of mixing and drying aluminum powder and silicon dioxide powder by using a high-energy ball mill under the protection of argon, adding the mixture into a smelted A356 alloy, standing the mixture for deslagging, and obtaining in-situ Al2O3A particulate reinforced aluminum matrix composite. Then adding rare earth element Ce into the in-situ Al by mechanical stirring2O3In the particle reinforced aluminum-based composite material, after the reaction is completed, the temperature is preserved, and the ultrafine grain aluminum-based composite material is prepared by pouring by utilizing a fluid director. The rare earth element Ce in the lanthanide series metal is the highest natural abundance metal in the lanthanide series metal, and has low price and good refining effect. The superfine crystal prepared by the method has simple process and low cost, and is suitable for large-scale productionAnd (4) production.
Description
Technical Field
The invention belongs to the technical field of ultra-fine grained aluminum alloy, and particularly relates to a method for preparing ultra-fine grained aluminum alloy by using a semi-solid forming technology.
Background
The A356 alloy has a series of excellent characteristics of good fluidity, small specific gravity, small hot cracking tendency and the like, and is widely applied to the industries of aerospace, automobiles and the like. With the development of aerospace technology, aluminum and aluminum alloy materials prepared by the traditional method are difficult to meet development requirements, and the microstructure of the aluminum and aluminum alloy materials needs to be further optimized to improve the mechanical properties of the aluminum and aluminum alloy materials. The semi-solid processing technology is a novel processing technology, has high production efficiency, can reduce porosity and has small impact on a casting mold, is beneficial to prolonging the service life of the mold, and thus has wide application prospect. The core of the semi-solid processing technology is to ensure that the prepared semi-solid alloy slurry has a non-dendritic fine and uniform spherical grain structure. The rare earth element is called as 'vitamin in the industry' and has the long-acting modification effects of refining alpha-Al dendrite, degassing and deslagging and refining eutectic silicon, and the modification effect of the rare earth has relative long-acting property and remelting stability, so that the rare earth element is an excellent modifier for the cast aluminum alloy at present. Research shows that the mechanical property of the block superfine crystal/nano crystal material prepared from aluminum and aluminum alloy can be effectively improved. At present, a severe plastic deformation method is mostly adopted for preparing the ultrafine-grained aluminum-silicon alloy, but in terms of the present, the severe plastic deformation process has complex processing process and higher cost, and large parts are very difficult to manufacture. Therefore, further research and improvement on the method for preparing the ultra-fine crystals are needed in various aspects.
Ce cerium is a periodic group III lanthanide, a rare earth element. Atomic number 58. A small amount of Ce is added into the aluminum alloy, so that grains can be well refined and various performances of the aluminum alloy can be improved. During the preparation of the Al-Ce intermediate alloy, the eutectic reaction generates alpha-Al and Al11Ce3. And Al11Ce3Has a certain coherent relation with Al, can be used as a heterogeneous nucleation core of the primary phase of the A356 alloy, and plays a role in refining grains. According to the existing literature, the Ce element is used for refining the semi-solid A356 aluminum alloy, the average diameter of the equal circle can be mostly refined to more than 30 micrometers, and the ultra-fine grain level cannot be achieved.
Disclosure of Invention
The invention aims to prepare the ultra-fine grain aluminum alloy by using a semi-solid forming technology. The mode for producing the ultra-fine grain overcomes the problem of difficult processing in the preparation of the ultra-fine grain aluminum alloy by a large plastic deformation process, and has lower cost.
The principle of the invention is as follows: rare earth elements Ce and Al as used herein2O3The grain size is further reduced by cooperating with the action of the flow guider. Al (Al)2O3Can be used as the core of heterogeneous nucleation. The rare earth Ce can also be used as a nucleation core and can promote Al2O3And (4) dispersing the particles. The Al-Ce reaction utilizes a grain refiner formed by self solidification of the aluminum-silicon alloy to meet the alloy solidification requirement in thermodynamics and kinetics, has no pollution to the alloy and the environment, and is a green and environment-friendly grain refining technology. Eutectic reaction of a1-Ce produced by Ce in a356 alloy: l → alpha-Al + Al11Ce3. The liquidus temperature of A356 is 615 deg.C, the eutectic temperature is 621 deg.C, the eutectic reaction occurs first and after solidification, the product of the eutectic reaction is alpha-Al and Al11Ce3Can be used as nucleation core when A356 alloy is solidified, thereby playing the role of refining the primary alpha-Al phase of the alloy. And (3) mechanically stirring by using a high-rotation-speed 800-plus-1200 r/min mechanical stirrer, crushing the alpha-Al dendrite, and controlling the heat preservation temperature and the heat preservation time, wherein a casting mold adopts a copper film, thereby further refining the grains. In the invention, the 45-degree inclined plate fluid director is adopted for pouring, the chilling effect is generated due to the lower temperature of the fluid director, a fine dendritic crystal solidified shell is formed on the surface of the fluid director, the root of the dendritic crystal is limited to grow to form necking grains due to solute segregation, the metal melt is separated from the surface of the fluid director under the action of shearing force to generate dissociation, and then the dendritic crystal on the surface layer of the solidified shell is broken or the solidified shell is completely separated from the wall of the fluid director and enters a die along with the metal melt under the action of liquid flow scouring, so that the nucleation rate is increased, and the grains are refined.
As an improvement of the technical scheme, the method comprises the following specific implementation steps:
step 1: and (2) mixing the following components in percentage by mass: 1 of Al and SiO2Putting the powder into a ball milling tank, ball milling and mixing for 4h under the protection of argon at the rotating speed of 250-350rpm, and drying the ground powder in a vacuum drying oven at the temperature of 100-150 ℃ for 2-4 h to obtain dried mixed powder(ii) a The addition amount of the mixed powder is such that Al in the finally prepared ultra-fine grained aluminum alloy2O3The volume percentage of the particles was 1%.
Preferably, 0.3% by mass of stearic acid based on the mass of the Al powder is added to the mixed powder to prevent cold welding.
Step 2: smelting A356 alloy in a graphite crucible, adding C with the mass of 0.4-0.6 wt% of the A356 alloy when the temperature is increased to 730-2Cl6Refining with refining agent, preferably 0.5 wt%, removing slag and standing for 2-10 min.
And step 3: and when the temperature is reduced to 590-610 ℃, adding the dried mixed powder into the melted A356 alloy vortex generated by mechanical stirring at 800-1200r/min, then mechanically stirring for 2-10min, raising the temperature to 800-900 ℃, and preserving the temperature for 30-40 min.
And 4, step 4: the fluid director needs to be placed in a drying box to be preheated to 200 ℃, and then ZnO coating is coated and dried. When the temperature is raised to 700-750 ℃, rare earth Ce accounting for 0.3-0.8 percent of the mass of the A356 alloy is added in the form of Al-20Ce intermediate alloy, preferably 0.5 percent, after the reaction is completed, the mixture is insulated for 1-2min in a 580-630 ℃ heat insulation control furnace, and then poured into a copper mold preheated for 2h at 200 ℃ by using a 45-degree inclined plate fluid director and rapidly quenched by water to obtain the ultrafine grain aluminum alloy.
Compared with the prior art, the invention has the following gain effects:
the rare earth element Ce is a very active silver gray metal and is the highest natural abundance in lanthanide metals. The purity is 99-99.9%, the market price is 35-45 yuan/kg, and the price is low. Al (Al)2O3Compared with a severe plastic deformation process, the method for preparing the ultra-fine grained aluminum alloy by using the semi-solid forming technology is simple in preparation process, low in price, excellent in performance and suitable for large-scale production.
Drawings
Fig. 1 is a deflector apparatus of embodiments 1, 2, 3;
FIG. 2 photograph of microstructure of aluminum alloy in example 1;
at this parameter, the matrix was not broken and coarse dendrites were present.
FIG. 3 photograph of microstructure of aluminum alloy in example 2;
at this parameter, the matrix dendrites are broken, but the matrix size is large and not round.
FIG. 4 photograph of microstructure of aluminum alloy in example 3.
The substrate prepared under the optimal process parameters is fine and round in size and can reach the grade of ultrafine crystals.
Detailed Description
The invention is further described with reference to the following examples and the accompanying drawings.
Example 1:
and (2) mixing the following components in percentage by mass: 1 of Al and SiO2The powder is put into a ball milling tank and is ball milled and mixed for 4 hours at the rotating speed of 250rpm under the protection of argon, and stearic acid accounting for 0.3 percent of the mass of the Al powder is added into the mixed powder to prevent cold welding. The milled powder was dried in a vacuum oven at 120 ℃ for 2 hours to obtain a dried mixed powder. Smelting A356 alloy in a graphite crucible, heating to 730 ℃, and adding C with the mass of 0.4 wt% of the A356 alloy2Cl6Refining with a refining agent, removing slag and standing for 5 min. And (3) slowly shaking the dried mixed powder by using a spoon and adding the mixed powder into the melted A356 alloy vortex by using 1000r/min mechanical stirring when the temperature is reduced to 610 ℃, mechanically stirring for 2min, heating to 900 ℃, and preserving the heat for 40 min. The fluid director needs to be placed in a drying box to be preheated to 200 ℃, and then ZnO coating is coated and dried. When the temperature is raised to 730 ℃, 0.3 percent of rare earth Ce is added in the form of Al-20Ce intermediate alloy, after the reaction is completed, the temperature is kept for 2min in a 630 ℃ heat preservation control furnace, and then the mixture is poured into a copper mould preheated at 200 ℃ for 2h by utilizing a 45-degree inclined plate fluid director and is rapidly quenched by water.
Example 2:
and (2) mixing the following components in percentage by mass: 1 of Al and SiO2The powder is put into a ball milling tank and is ball milled and mixed for 4 hours at the rotating speed of 250rpm under the protection of argon, and stearic acid accounting for 0.3 percent of the mass of the Al powder is added into the mixed powder to prevent cold welding. The milled powder was dried in a vacuum oven at 120 ℃ for 2 hours to obtain a dried mixed powder. Smelting A356 alloy in a graphite crucible, heating to 730 ℃, and adding C with the mass of 0.4 wt% of the A356 alloy2Cl6Refining agent for refining and removing molten metalSlag and standing for 2 min. And (3) slowly shaking the dried mixed powder by using a spoon and adding the mixed powder into the melted A356 alloy vortex by using 1200r/min mechanical stirring when the temperature is reduced to 610 ℃, mechanically stirring for 5min, heating to 850 ℃, and keeping the temperature for 30 min. The fluid director needs to be placed in a drying box to be preheated to 200 ℃, and then ZnO coating is coated and dried. When the temperature is raised to 730 ℃, 0.8 percent of rare earth Ce is added in the form of Al-20Ce intermediate alloy, after the reaction is completed, the temperature is kept for 2min in a 630 ℃ heat preservation control furnace, and then the mixture is poured into a copper mould preheated at 200 ℃ for 2h by utilizing a 45-degree inclined plate fluid director and is rapidly quenched by water.
Example 3:
and (2) mixing the following components in percentage by mass: 1 of Al and SiO2The powder is put into a ball milling tank and is ball milled and mixed for 4 hours at the rotating speed of 250rpm under the protection of argon, and stearic acid accounting for 0.3 percent of the mass of the Al powder is added into the mixed powder to prevent cold welding. The milled powder was dried in a vacuum oven at 120 ℃ for 2 hours to obtain a dried mixed powder. Smelting A356 alloy in a graphite crucible, heating to 740 ℃, and adding C with the mass of 0.5 wt% of the A356 alloy2Cl6Refining with a refining agent, removing slag and standing for 5 min. And (3) slowly shaking the dried mixed powder by using a spoon and adding the mixed powder into the melted A356 alloy vortex by using 1200r/min mechanical stirring when the temperature is reduced to 600 ℃, mechanically stirring for 8min, heating to 850 ℃, and preserving the temperature for 30 min. The fluid director needs to be placed in a drying box to be preheated to 200 ℃, and then ZnO coating is coated and dried. When the temperature is increased to 710 ℃, 0.5 percent of rare earth Ce is added in the form of Al-20Ce intermediate alloy, after the reaction is completed, the temperature is kept for 1min in a 610 ℃ heat preservation control furnace, and then the mixture is poured into a copper mould preheated at 200 ℃ for 2h by utilizing a 45-degree inclined plate fluid director and is rapidly quenched by water.
Claims (6)
1. A method for preparing ultra-fine grain aluminum alloy by using a semi-solid forming technology is characterized by comprising the following specific steps:
step 1: mixing Al and SiO2Putting the powder into a ball milling tank, ball milling and mixing under the protection of argon, and drying the milled powder to obtain mixed powder; the addition amount of the mixed powder is such that Al in the finally prepared ultra-fine grained aluminum alloy2O3The volume percentage of the particles is 1%；
Step 2: smelting A356 alloy in a graphite crucible, adding C with the mass of 0.4-0.6 wt% of the A356 alloy when the temperature is increased to 730-2Cl6Refining by using a refining agent, removing slag and standing;
and step 3: when the temperature is reduced to 590-610 ℃, adding the dried mixed powder into the melted A356 alloy vortex generated by applying mechanical stirring, then mechanically stirring for 2-10min, heating to 800-900 ℃, and preserving the heat for 30-40 min;
and 4, step 4: when the temperature is raised to 700-750 ℃, rare earth Ce accounting for 0.3-0.8% of the mass of the A356 alloy is added, after the reaction is completed, the temperature is kept for 1-2min in a 580-630 ℃ heat preservation control furnace, and then the mixture is poured into a die by utilizing a 45-degree inclined plate fluid director and is rapidly water-quenched to obtain the ultra-fine grain aluminum alloy.
2. The method for preparing ultra-fine grained aluminum alloy by using semi-solid forming technology as claimed in claim 1, wherein in step 1, the rotation speed of ball milling and mixing is 250-350rpm for 4 hours; al and SiO2The mass ratio of the powder is 2: 1; drying refers to drying in a vacuum drying oven at 100 ℃ and 150 ℃ for 2-4 hours.
3. The method for preparing an ultra-fine grained aluminum alloy using a semi-solid forming technique according to claim 1, wherein in step 1, stearic acid is added to the mixed powder in an amount of 0.3% by mass of the Al powder to prevent cold welding.
4. The method for preparing an ultra-fine grained aluminum alloy using a semi-solid forming technique according to claim 1, wherein in step 2, C is2Cl6The adding amount of the refining agent is 0.5 percent of the mass of the A356 alloy; standing for 2-10 min.
5. The method for preparing ultra-fine grained aluminum alloy by using semi-solid forming technology as claimed in claim 1, wherein the rotation speed of the mechanical stirring in step 3 is 800-1200 r/min.
6. The method for preparing ultra-fine grained aluminum alloy by using the semi-solid forming technology as claimed in claim 1, wherein in the step 4, the fluid director is placed in a drying oven to be preheated to 200 ℃, and then coated with ZnO coating and dried; the addition mode of the rare earth Ce is in the form of Al-20Ce intermediate alloy, and the addition amount is 0.5 percent of the mass of the A356 alloy; the die is a copper die, and the copper die needs to be preheated for 2 hours at 200 ℃.
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| CN115074571A (en) * | 2022-06-28 | 2022-09-20 | 江苏大学 | Method for preparing in-situ particle reinforced aluminum-based composite material by semi-solid technology |
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