CN110343895B - In situ TiB2Preparation method of particle-reinforced AlCu-based composite material - Google Patents
In situ TiB2Preparation method of particle-reinforced AlCu-based composite material Download PDFInfo
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- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
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- C22C21/12—Alloys based on aluminium with copper as the next major constituent
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
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Abstract
Hair brushRelates to the technical field of aluminum-copper alloy, in particular to in-situ TiB2The preparation method of the particle reinforced AlCu-based composite material has low preparation cost, can realize macro-production, adopts high-energy ball milling to refine and fully mix the mixed salt and press the mixed salt into a precast block, melts the precast block into the molten metal in a layer-by-layer peeling mode during the reaction, enlarges the contact area of the mixed salt and the molten metal, ensures the component proportion of the reaction salt, improves the reaction efficiency, reduces the reaction difficulty and improves the yield of reaction elements; the electromagnetic stirring aggravates the convection in the melt, causes the strong scouring of the liquid-solid interface, and forms cluster TiB in the melt2The particles are broken down by the high-speed flowing liquid flow, become smaller in size and are uniformly distributed in the melt under strong electromagnetic stirring.
Description
Technical Field
The invention relates to the technical field of aluminum-copper alloy, in particular to in-situ TiB2A preparation method of a particle reinforced AlCu-based composite material.
Background
The aluminum-based composite material has the advantages of light weight, wear resistance, corrosion resistance, low thermal expansion coefficient and the like, and gradually becomes the key direction of high-performance material research in the fields of aviation, aerospace, automobiles, electronics and other industries; compared with the traditional external method, the in-situ self-generation TiB2The particle reinforced aluminum matrix composite has the characteristics of high specific strength and rigidity, small anisotropy, high elastic modulus, good bonding with an aluminum alloy matrix interface and the like, and has become a hot problem in the research field of aluminum matrix composites; at present, the existing TiB2The low yield of reaction elements and iB still exist in the preparation process of the particle reinforced aluminum-based composite material2Uneven distribution, agglomeration and TiB of reinforcement2Large particle size, high preparation cost, difficult realization of macro-production and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an in-situ TiB2The preparation method of the particle-reinforced AlCu-based composite material specifically comprises the following steps:
(1) mixing potassium fluoborate and potassium fluotitanate, performing high-energy ball milling, adding industrial alcohol, mixing, pressing into a cylindrical precast block, and then placing into a 200-300 ℃ oven for heat preservation for 3-4 hours to obtain a cured mixed salt precast block;
(2) and pressing the solidified mixed salt prefabricated block into the bottom of the molten metal in the crucible of the electromagnetic induction furnace by using a long-handle graphite spoon to perform full reaction.
Further, the atomic ratio of Ti and B in the potassium fluoroborate and the potassium fluorotitanate is 1: 2.
further, the rotation speed of the ball milling is 100-.
Further, the mass percentages of the elements in the molten metal are as follows: 4.6-5.3% of Cu, 0.3-0.5% of Mn, 0.15-0.3% of Ti, 0.15-0.25% of Cd, 0.10-0.30% of Zr, 0.005-0.06% of B, 0.10-0.30% of V, 0.01-0.2% of Y and the balance of Al.
Further, the density of the pressed precast block is 65-75%.
Furthermore, the specification of the precast block is (phi 50-phi 80) mm x (50-100) mm.
Further, the molten metal raw materials comprise a refined aluminum ingot, an aluminum-copper intermediate alloy, an aluminum-manganese intermediate alloy, metal cadmium, an aluminum-vanadium intermediate alloy, an aluminum-zirconium intermediate alloy, an aluminum-titanium-boron intermediate alloy and an aluminum-yttrium intermediate alloy.
Further, the preparation of the molten metal specifically comprises the following steps: preheating a smelting crucible to the temperature of 300-.
The invention adopts a mixed salt reaction method to prepare the composite material by in-situ synthesis, and the reaction equation is as follows: 3K2TiF6+6KBF4+10Al＝3TiB2+9KAlF4+K3AlF6。
Advantageous effects
The invention adopts high-energy ball milling to refine and fully mix the mixed salt and press the mixed salt into the precast block, and the precast block is melted into the molten metal in a mode of peeling layer by layer during the reaction, thereby enlarging the contact area of the mixed salt and the molten metal, ensuring the component proportion of the reaction salt, improving the reaction efficiency, reducing the reaction difficulty and further ensuring the high yield of reaction elements; the electromagnetic stirring aggravates the convection in the melt, causes the strong scouring of the liquid-solid interface, and forms cluster TiB in the melt2The particles are broken down by the high-speed flowing liquid flow, become smaller in size and are uniformly distributed in the melt under strong electromagnetic stirring.
TiB prepared by the invention2The particle-reinforced AlCu-based composite material has the advantages that particles are uniformly distributed, the particle size is small, the tissue distribution is uniform, the tensile strength is improved by 10-15% compared with that of a matrix alloy, and the yield strength is improved by 15-20%; the invention has simple process, low manufacturing cost and high yield of reaction elements, can directly prepare the composite material cast ingot by casting in a smelting mode, can also prepare a casting by combining the preparation of the composite material with sand mold and metal mold casting, and is suitable for industrialized mass production.
Drawings
FIG. 1 is a schematic illustration of the preparation of a composite material of the present invention;
FIG. 2 is a metallographic structure of a composite material prepared according to the present invention;
Detailed Description
The technical solution of the present invention is further limited by the following specific embodiments, but the scope of the claims is not limited to the description.
Example 1
In-situ TiB2The preparation method of the particle-reinforced AlCu-based composite material specifically comprises the following steps:
(1) mixing potassium fluoborate and potassium fluotitanate, performing high-energy ball milling, wherein the ball milling rotation speed is 100r/min, the ball milling time is 5min, adding industrial alcohol after the ball milling is finished, pressing into a cylindrical precast block with the specification of phi 5 multiplied by 50mm and the density of 65%, and then putting the cylindrical precast block into a 200 ℃ oven for heat preservation for 3h to obtain a solidified mixed salt precast block;
(2) preheating a smelting crucible to 300 ℃, preserving heat for 2 hours, adding a refined aluminum ingot, an aluminum-copper intermediate alloy and an aluminum-manganese intermediate alloy, heating to melt the refined aluminum ingot, the aluminum-copper intermediate alloy and the aluminum-manganese intermediate alloy, stirring for 1min, heating to 680 ℃, adding metal cadmium and the aluminum-zirconium intermediate alloy, stirring for 1min after melting, heating to 700 ℃, adding the aluminum-vanadium intermediate alloy, stirring for 1min after melting, adjusting the temperature to 700 ℃, adding the aluminum-titanium-boron intermediate alloy and the aluminum-yttrium intermediate alloy, stirring for 3min after melting, heating to 850 ℃ to obtain molten metal, pressing a solidified mixed salt prefabricated block into the bottom of an electromagnetic induction furnace crucible filled with the molten metal by using a long-handle graphite spoon until the depth of the molten metal reaches 2/3 of the molten metal solution, scooping out a surface layer molten salt by using a skimming spoon after the reaction is completed (no spark appears on the surface of the molten alloy liquid), standing for 15min at 880 ℃, adjusting the melt to 710 ℃, refining, pouring into a preheated metal mold or casting.
Further, the atomic ratio of Ti and B in the potassium fluoroborate and the potassium fluorotitanate is 1: 2.
further, the mass percentages of the elements in the molten metal are as follows: 4.6% of Cu, 0.3% of Mn, 0.15% of Ti, 0.15% of Cd, 0.10% of Zr, 0.005% of B, 0.10% of V, 0.01% of Y and the balance of Al.
Example 2
In-situ TiB2The preparation method of the particle-reinforced AlCu-based composite material specifically comprises the following steps:
(1) mixing potassium fluoborate and potassium fluotitanate, performing high-energy ball milling at the rotating speed of 100-400r/min for 5-100min, adding industrial alcohol after the ball milling is finished, pressing into cylindrical precast blocks with the specification of phi 80 multiplied by 100mm and the density of 75%, and then putting the cylindrical precast blocks into a 300 ℃ drying oven for heat preservation for 4 hours to obtain cured mixed salt precast blocks;
(2) preheating a smelting crucible to 500 ℃, preserving heat for 4 hours, adding refined aluminum ingot, aluminum copper intermediate alloy and aluminum manganese intermediate alloy, heating to melt the refined aluminum ingot, aluminum copper intermediate alloy and aluminum manganese intermediate alloy, stirring for 3 minutes, heating to 700 ℃, adding metal cadmium and aluminum zirconium intermediate alloy, stirring for 3 minutes after melting, heating to 730 ℃, adding aluminum vanadium intermediate alloy, stirring for 3 minutes after melting, adjusting the temperature to 750 ℃, adding aluminum titanium boron intermediate alloy and aluminum yttrium intermediate alloy, stirring for 5 minutes after melting, heating to 900 ℃ again to obtain molten metal, pressing a solidified mixed salt precast block into the bottom of an electromagnetic induction furnace crucible filled with the molten metal by using a long-handle graphite spoon until the depth of the molten metal is 2/3, scooping out a surface molten salt by using a skimming spoon after complete reaction, standing at 900 deg.C for 20min, adjusting melt to 730 deg.C, refining with high purity argon gas for 20min, standing for 10min, and pouring into preheated metal mold or casting.
Further, the atomic ratio of Ti and B in the potassium fluoroborate and the potassium fluorotitanate is 1: 2.
further, the mass percentages of the elements in the molten metal are as follows: 5.3% of Cu, 0.5% of Mn, 0.3% of Ti, 0.25% of Cd, 0.30% of Zr, 0.06% of B, 0.10-0.30% of V, 0.2% of Y and the balance of Al.
Example 3
In-situ TiB2The preparation method of the particle-reinforced AlCu-based composite material specifically comprises the following steps:
(1) mixing potassium fluoborate and potassium fluotitanate, performing high-energy ball milling, wherein the ball milling rotation speed is 150r/min, the ball milling time is 20min, adding industrial alcohol after the ball milling is finished, pressing into a cylindrical precast block with the specification of phi 50 multiplied by 60mm and the density of 70%, and then putting the cylindrical precast block into a 250 ℃ oven for heat preservation for 3h to obtain a solidified mixed salt precast block;
(2) preheating a smelting crucible to 400 ℃, preserving heat for 3 hours, adding a refined aluminum ingot, an aluminum-copper intermediate alloy and an aluminum-manganese intermediate alloy, heating to melt the refined aluminum ingot, the aluminum-copper intermediate alloy and the aluminum-manganese intermediate alloy, stirring for 2 minutes, heating to 690 ℃, adding metal cadmium and the aluminum-zirconium intermediate alloy, stirring for 2 minutes after melting, heating to 715 ℃, adding the aluminum-vanadium intermediate alloy, stirring for 2 minutes after melting, adjusting the temperature to 725 ℃, adding the aluminum-titanium-boron intermediate alloy and the aluminum-yttrium intermediate alloy, stirring for 5 minutes after melting, heating to 880 ℃ again to obtain molten metal, pressing a solidified mixed salt prefabricated block into the bottom of an electromagnetic induction furnace crucible filled with the molten metal by using a long-handle graphite spoon until the molten metal reaches 2/3 of the depth of the molten metal, scooping out a surface layer molten salt by using a skimming spoon after complete reaction (no spark appears on the surface of the molten alloy), standing for 20 minutes at 880-900 ℃, adjusting the melt to 720 ℃, standing for 8min, and pouring into preheated metal mold or casting.
Further, the atomic ratio of Ti and B in the potassium fluoroborate and the potassium fluorotitanate is 1: 2.
further, the mass percentages of the elements in the molten metal are as follows: 5.0% Cu, 0.4% Mn, 0.25% Ti, 0.20% Cd, 0.20% Zr, 0.005% B, 0.20% V, 0.01% Y, the balance Al.
It should be noted that the above examples and test examples are only for further illustration and understanding of the technical solutions of the present invention, and are not to be construed as further limitations of the technical solutions of the present invention, and the invention which does not highlight essential features and significant advances made by those skilled in the art still belongs to the protection scope of the present invention.
Claims (6)
1. In situ TiB2The preparation method of the particle-reinforced AlCu-based composite material is characterized by comprising the following steps of: (1) mixing potassium fluoborate and potassium fluotitanate, performing high-energy ball milling, adding industrial alcohol, mixing, pressing into a cylindrical precast block, and then placing into a 200-300 ℃ oven for heat preservation for 3-4 hours to obtain a cured mixed salt precast block; (2) pressing the solidified mixed salt prefabricated block into the bottom of molten metal in a crucible of an electromagnetic induction furnace by using a long-handle graphite spoon to perform full reaction;
the rotation speed of the ball milling is 100-;
the mass percentages of all elements in the molten metal are as follows: 4.6-5.3% of Cu, 0.3-0.5% of Mn, 0.15-0.3% of Ti, 0.15-0.25% of Cd, 0.10-0.30% of Zr, 0.005-0.06% of B, 0.10-0.30% of V, 0.01-0.2% of Y and the balance of Al.
2. As in claimClaim 1 the in situ TiB2The preparation method of the particle-reinforced AlCu-based composite material is characterized in that the atomic ratio of Ti to B in the potassium fluoborate to the potassium fluotitanate is 1: 2.
3. the in situ TiB of claim 12The preparation method of the particle-reinforced AlCu-based composite material is characterized in that the compactness of the pressed precast block is 65-75%.
4. The in situ TiB of claim 12The preparation method of the particle-reinforced AlCu-based composite material is characterized in that the specification of the precast block is (phi 50-phi 80) mmx (50-100) mm.
5. The in situ TiB of claim 12The preparation method of the particle reinforced AlCu-based composite material is characterized in that the molten metal raw materials comprise a refined aluminum ingot, an aluminum-copper intermediate alloy, an aluminum-manganese intermediate alloy, metal cadmium, an aluminum-vanadium intermediate alloy, an aluminum-zirconium intermediate alloy, an aluminum-titanium-boron intermediate alloy and an aluminum-yttrium intermediate alloy.
6. The in situ TiB of claim 1 or 52The preparation method of the particle-reinforced AlCu-based composite material is characterized in that the preparation of the molten metal specifically comprises the following steps: preheating a smelting crucible to the temperature of 300-.
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