CN113373367A - Aluminum intermediate alloy containing multi-scale mixed particles and preparation method thereof - Google Patents
Aluminum intermediate alloy containing multi-scale mixed particles and preparation method thereof Download PDFInfo
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- CN113373367A CN113373367A CN202110622822.3A CN202110622822A CN113373367A CN 113373367 A CN113373367 A CN 113373367A CN 202110622822 A CN202110622822 A CN 202110622822A CN 113373367 A CN113373367 A CN 113373367A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- 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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- 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
Abstract
The invention belongs to the field of non-ferrous metal material preparation, and particularly relates to an aluminum intermediate alloy containing multi-scale mixed particles and a preparation method thereof2TiF6、KBF4、KCl、BaCl2Pouring the mixed salt into the aluminum melt, and carrying out in-situ reaction in the aluminum melt to generate submicron TiB2Particles, nano TiC particle fused salt is precipitated into the aluminum melt in an auxiliary mode, and the submicron TiB with uniform dispersion distribution is prepared in a vibration external field dispersion mode2The process is simple, the preparation efficiency is high, the method is suitable for large-scale industrial production of the multi-scale mixed particle modified aluminum alloy material, the solidified grain structure of the aluminum alloy can be obviously refined, and the aluminum alloy solidification hot cracks are reducedHas good popularization value.
Description
Technical Field
The invention belongs to the field of preparation of non-ferrous metal materials, and particularly relates to an aluminum intermediate alloy containing multi-scale mixed particles and a preparation method thereof.
Background
Some simple substances are made into alloy, so that the alloy is convenient to be added into the alloy, the problems of burning loss, difficult melting of high-melting point alloy and the like are solved, and the special alloy which has little influence on raw materials is called intermediate alloy.
The aluminum alloy has the advantages of good electrical and thermal conductivity, high strength-to-mass ratio, corrosion resistance, damage resistance and the like, is widely applied to the fields of aerospace, rail transit, automobiles, ships, pressure vessels, electronic and electric appliances, furniture and the like, and is one of the most widely applied metal materials in the industry at present.
The application number of CN201210572236.3 discloses a process for refining pure aluminum by using Al-5% Ti-1% B intermediate alloy. The method mainly comprises the following steps: 1) performing equal channel deformation on the Al-5% Ti-1% B intermediate alloy at room temperature; 2) putting the ceramic crucible containing the aluminum ingot and the refining agent into a shaft furnace, and heating to 760 ℃ to melt the ceramic crucible; 3) adding an equal-channel deformed Al-5% Ti intermediate alloy which accounts for 0.2-0.6% of the weight of pure aluminum into the aluminum liquid; 4) stirring and heating the aluminum liquid, and standing for 5-60 minutes; 5) pouring the aluminum liquid into an iron mold at the temperature of 720-800 ℃, demolding, and cooling to room temperature by water. According to the technical scheme of the refining process, the fine blocky TiAl3 and TiB2 in the Al-5% Ti-1% B intermediate alloy are used as effective heterogeneous nucleation cores, the nucleation rate of a melt is improved, so that grains are refined, the grain size of an industrial pure aluminum ingot can be refined to be less than 100 mu m, the isometric crystal area range is remarkably expanded, and better comprehensive physical and mechanical properties are obtained.
According to the scheme, the smelting temperature of the aluminum intermediate alloy is not more than 800 ℃, the aluminum alloy is manufactured by the aluminum intermediate alloy and the reinforcements, the performance of the aluminum alloy material depends on the characteristics, the content, the distribution and other factors of the base alloy and the reinforcements, the thermal expansion coefficients of a plurality of reinforcements are small, the difference between the thermal conductivity, the linear expansion coefficient and other thermophysical properties of the two reinforcements is large, and the aluminum alloy 3D printing material is easy to generate hot cracks in the welding or 3D printing process.
Disclosure of Invention
The invention provides an aluminum intermediate alloy of multi-scale mixed particles and a preparation method thereof, wherein the aluminum intermediate alloy can obviously refine an aluminum alloy solidification structure and obviously reduce the hot crack sensitivity of the aluminum alloy solidification structure.
In order to achieve the above object, the present invention provides a multi-scale mixed particle aluminum master alloy characterized by containing submicron TiB20.1-6.4% of particles; 0.1-3% of nano TiC particles; the balance being aluminum and impurities.
The principle of the scheme is as follows: addition of nano-submicron multi-scale TiC particles and TiB to aluminum master alloy2The grains are added with the compound addition of various grains, so that grains can be obviously refined, and the hot crack sensitivity of the aluminum alloy material is reduced. When micron-scale and nano-scale ceramic particles are introduced simultaneously, a synergistic effect is generated among different-scale particles, so that the rigidity and toughness of the aluminum intermediate alloy are improved, and the hot crack sensitivity of the aluminum alloy material is reduced.
The scheme has the beneficial effects that: by adding composite particles of nano and submicron particles, the content of the composite particles is controllable, the particles with different sizes are mixed with a grain enhancer, and the mutual cooperation among the particles with different sizes improves the performance of the aluminum intermediate alloy, so that the interface combination of a matrix is good, the particles are distributed and dispersed, and the modification effect is excellent; the aluminum alloy material prepared by the aluminum intermediate alloy containing the multi-scale mixed particles can obviously refine the aluminum alloy solidification grain structure and reduce the aluminum alloy solidification hot cracks due to the existence of the multi-scale mixed particles, and simultaneously can improve the strength performance of the aluminum alloy material, and has great advantages in the preparation of aluminum alloy structure materials, the improvement of high-strength alloy hot crack sensitivity and the like.
Further, it is characterized byThe submicron TiB2The mass percent of the particles is 3.2 percent; the mass percentage of the nano TiC particles is 2%; the balance being aluminum and impurities.
Further, the submicron TiB2The particles are generated by adopting an in-situ reaction; and the nano TiC particles are precipitated into the aluminum melt in a molten salt auxiliary mode.
In order to achieve the aim, the invention provides a method for preparing an aluminum intermediate alloy with multi-scale mixed particles, which is to uniformly mix K of nano TiC particles2TiF6、KBF4、KCl、BaCl2The mixed salt reacts in situ in the aluminum melt to generate submicron TiB2 particles, meanwhile, the nano TiC particle molten salt is precipitated into the aluminum melt in an auxiliary mode, and then the aluminum intermediate alloy containing the submicron TiB2 and the nano TiC multi-scale mixed particles which are uniformly dispersed and distributed is prepared in a vibration external field dispersion mode.
The preparation method of the aluminum intermediate alloy has the advantages of simple process, high preparation efficiency and the like, is suitable for large-scale industrial production of the aluminum matrix composite, and has good popularization value.
Further, the specific process steps are as follows: step 1: preparing K according to the proportion2TiF6、KBF4、KCl、BaCl2Mixing salt; step 2: uniformly mixing the nano TiC particles with the mixed salt; and step 3: placing the graphite crucible into a smelting furnace, placing pure aluminum into the graphite crucible, and starting the smelting furnace to heat the graphite crucible to enable the temperature in the graphite crucible to reach 780 ℃ so as to melt the pure aluminum; and 4, step 4: pouring the mixed salt with the uniformly mixed nano particles into the aluminum melt; and 5: heating the aluminum melt to 800-850 ℃; step 6: uniformly stirring the aluminum melt for 15-30 minutes; and 7: taking the crucible containing the aluminum melt out of the smelting furnace, placing the crucible on a high-frequency vibrating plate, and naturally cooling; and 8: and after the melt is completely cooled, removing the salt on the surface to obtain the aluminum intermediate alloy with the multi-scale mixed particles. Submicron TiB2The particles and the nano TiC particles have better wettability with aluminum within the temperature range of 800-850 ℃.
Further, K is2TiF6And KBF4The mass ratio of (A) to (B) is 0.9 to 1.0.
Further, the nano TiC particles and K2TiF6、KBF4、KCl、BaCl2The mass ratio of the mixed salt is 1: 7-1: 10.
Further, in the step 6, the aluminum melt is uniformly stirred in an electromagnetic stirring mode. The particles can be settled as much as possible, and the particles are uniformly distributed.
Further, in the step 6, the aluminum melt is uniformly stirred by adopting an electrically controlled mechanical stirring mode with a propeller type stirring head, and the rotating speed of the stirring head is 150-250 rmp/min. The particles can be settled as much as possible, and the particles are uniformly distributed.
Drawings
FIG. 1 is a schematic diagram of the smelting preparation principle of the invention.
FIG. 2 is an SEM image of an Al master alloy material containing gradient TiB2 and TiC composite particles prepared by the invention.
Fig. 3 is a gold phase diagram of a 7075 aluminum alloy prepared from pure aluminum.
Fig. 4 is a gold phase diagram of 7075 aluminum alloy prepared with the Al master alloy of comparative example 1 containing only TiB2 particles.
Fig. 5 is a diagram of the gold phase of 7075 aluminum alloy prepared from the Al master alloy containing multi-scale mixed particles prepared by the invention.
Detailed Description
The following is further detailed by the specific embodiments:
reference numerals in the drawings of the specification include: smelting furnace 1, graphite crucible 2 and TiB2Particles 3, TiC particles 4, mixed salt 5 and aluminum melt 6.
Example 1:
an aluminum master alloy containing multi-scale mixed particles contains 0.1-6.4% by mass of 3 submicron TiB2 particles (in this embodiment, 3 submicron TiB2 particles is 6.4% by mass); the mass percentage of the nano TiC particles 4 is 0.1-3% (in the embodiment, the nano TiC particles 4 are 1%); the balance being aluminum and impurities.
The impurities described in this example are unavoidable, mainly in the case of the alloy being smelted, just as the difference in toughness due to the difference in carbon content between the steel and the pig iron is also the only difference, and are therefore said to be unavoidable. As shown in the attached figure 1, the device for preparing the aluminum master alloy containing the multi-scale mixed particles comprises a smelting furnace 1 and a graphite crucible 2, wherein the smelting furnace 1 is used for heating the graphite crucible 2.
A preparation method of an aluminum master alloy containing multi-scale mixed particles comprises the following steps:
step 1: preparing K according to the proportion2TiF6、KBF4、KCl、BaCl2Mixed salt 5 (K)2TiF6And KBF4Mass ratio of (1) is 0.9 to 1.0), K in example 12TiF6And KBF4Is 0.92;
step 2: nano TiC particles 4 and mixed salt 5 (nano TiC particles 4 and K)2TiF6、KBF4、KCl、BaCl2The mass ratio of the mixed salt 5 is controlled to be 1: 7-1: 10), in this embodiment, the nano TiC particles 4 and K are uniformly mixed2TiF6、KBF4、KCl、BaCl2The mass ratio of the mixed salt 5 is 1: 8;
and step 3: placing the graphite crucible 2 into a smelting furnace 1, placing pure aluminum into the graphite crucible 2, starting the smelting furnace 1 to heat the graphite crucible 2, and enabling the temperature in the graphite crucible 2 to reach 780 ℃ to melt the pure aluminum;
and 4, step 4: pouring the mixed salt 5 with the uniformly mixed nano particles into an aluminum melt 6;
and 5: heating the aluminum melt 6 to 800-850 ℃ (submicron TiB)2The particles 3 and the nano TiC particles 4 have good wettability with aluminum within the temperature range of 800-850 ℃, so that the interface of the aluminum intermediate alloy matrix is well combined, the particles are distributed and dispersed, and the modification effect is excellent. ) In the embodiment, the temperature of the aluminum melt 6 is increased to 820 ℃;
step 6: uniformly stirring the aluminum melt for 6 minutes, 15-30 minutes, wherein the time for stirring the aluminum melt for 6 minutes in the embodiment is 30 minutes;
and 7: taking the graphite crucible 2 filled with the aluminum melt 6 out of the smelting furnace 1, placing the graphite crucible on a high-frequency vibrating plate, and naturally cooling;
and 8: after the melt is completely cooled, the surface salt is removed, and the aluminum master alloy of the multi-scale mixed particles can be obtained, as shown in fig. 2, it can be seen that particles with different sizes exist in the SEM image of the aluminum master alloy of the multi-scale mixed particles obtained by the method.
Example 2:
the difference between the aluminum master alloy and the embodiment 1 is that the aluminum master alloy contains 3 mass percent of submicron TiB2 particles, namely 3.2 percent; the mass percent of the nano TiC particles 4 is 2 percent; the balance being aluminum and impurities.
Example 3:
the difference between the aluminum master alloy and the embodiment 1 is that the aluminum master alloy contains 2.9 percent of submicron TiB2 particles 3 by mass; the mass percent of the nano TiC particles 4 is 1.5 percent; the balance being aluminum and impurities.
Example 4:
this example is different from example 1 in that the stirring is performed in step 6 by an electromagnetic stirring method or an electrically controlled mechanical stirring method with a propeller-type stirring head, and the other conditions are the same. The rotating speed of the stirring head is 150-250 rmp/min. The melt in the liquid cavity is stirred by a mechanical or electromagnetic induction method, so that the submicron TiB2 particles 3 and the nanometer TiC particles 4 can be settled as much as possible, and the particles are uniformly distributed.
Comparative example 1:
comparative example 1 differs from example 2 in that the aluminum master alloy has no nano TiC particles 4 added thereto, and the rest of the conditions are the same.
For the sake of easy visual comparison, the components and contents of examples 1 to 3 and comparative example 1, excluding aluminum, are tabulated as shown in table 1:
the aluminum alloy materials are prepared by using the aluminum master alloy materials and the reinforcers produced by all the examples and the comparative examples under the same preparation conditions.
The aluminum alloy prepared by the material produced in the comparative example 1 is not added with TiC particles 4, so that the solidification grain structure of the aluminum alloy is still a dendritic crystal structure, and the solidification thermal cracking of the aluminum alloy is high.
FIG. 3 is a photograph of a gold phase of 7075 aluminum alloy prepared from pure aluminum, and FIG. 4 is a photograph of a gold phase of a 7075 aluminum alloy prepared from comparative example 1 containing only TiB2FIG. 5 is a gold phase diagram of 7075 aluminum alloy prepared from Al master alloy containing multi-scale mixed particles prepared in example 2 of the present invention, and FIG. 4 and FIG. 3 show that the grain structure of aluminum alloy prepared from the Al master alloy in comparative example 1 is finer than that of aluminum alloy prepared from pure aluminum, and TiB2The particles can refine the grain structure and reduce the solidification hot cracks of the aluminum alloy. As shown in attached figures 4 and 5, the grain structure of the aluminum alloy material prepared from the aluminum master alloy in the sampling comparative example 1 is finer than that of the aluminum alloy material prepared from the aluminum master alloy in the embodiment 2, and the attached figures 3, 4 and 5 can prove that the multi-scale mixed particles can obviously refine the aluminum alloy solidification grain structure under the synergistic effect, reduce the aluminum alloy solidification hot cracks, improve the strength performance of the aluminum alloy material, and have great advantages in the aspects of preparation of the aluminum alloy structure material, improvement of high-strength alloy hot crack sensitivity and the like. The method has the advantages of simple process, high preparation efficiency and the like, is suitable for large-scale industrial production of the multi-scale mixed particle modified aluminum alloy material, and has good popularization value.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (9)
1. An aluminum master alloy containing multi-scale mixed particles, which is characterized in that: containing submicron TiB2The mass percentage of the particles is 0.1-6.4%; the mass percentage of the nano TiC particles is 0.1-3%; the balance being aluminum and impurities.
2. The aluminum master alloy containing multi-scale mixed particles as claimed in claim 1, wherein: the submicron TiB2The mass percent of the particles is 3.2 percent; the mass percentage of the nano TiC particles is 2%; the balance being aluminum and impurities.
3. The aluminum master alloy containing multi-scale mixed particles as claimed in claim 1, wherein: the submicron TiB2The particles are generated by adopting an in-situ reaction; and the nano TiC particles are precipitated into the aluminum melt in a molten salt auxiliary mode.
4. A preparation method of an aluminum intermediate alloy containing multi-scale mixed particles is characterized by comprising the following steps: k of evenly mixed nano TiC particles2TiF6、KBF4、KCl、BaCl2The mixed salt reacts in situ in the aluminum melt to generate submicron TiB2 particles, meanwhile, the nano TiC particle molten salt is precipitated into the aluminum melt in an auxiliary mode, and then the aluminum intermediate alloy containing the submicron TiB2 and the nano TiC multi-scale mixed particles which are uniformly dispersed and distributed is prepared in a vibration external field dispersion mode.
5. The method for preparing the aluminum master alloy containing the multi-scale mixed particles as claimed in claim 4, wherein the method comprises the following steps: the specific process steps are as follows:
step 1: preparing K according to the proportion2TiF6、KBF4、KCl、BaCl2Mixing salt;
step 2: uniformly mixing the nano TiC particles with the mixed salt;
and step 3: placing the graphite crucible into a smelting furnace, placing pure aluminum into the graphite crucible, and starting the smelting furnace to heat the graphite crucible to enable the temperature in the graphite crucible to reach 780 ℃ so as to melt the pure aluminum;
and 4, step 4: pouring the mixed salt with the uniformly mixed nano particles into the aluminum melt;
and 5: heating the aluminum melt to 800-850 ℃;
step 6: uniformly stirring the aluminum melt for 15-30 minutes;
and 7: taking the crucible containing the aluminum melt out of the smelting furnace, placing the crucible on a high-frequency vibrating plate, and naturally cooling;
and 8: and after the melt is completely cooled, removing the salt on the surface to obtain the aluminum intermediate alloy with the multi-scale mixed particles.
6. The method for preparing an aluminum master alloy containing multi-scale mixed particles as claimed in claim 4 or 5, wherein: said K2TiF6And KBF4The mass ratio of (A) to (B) is 0.9 to 1.0.
7. The method for preparing an aluminum master alloy containing multi-scale mixed particles as claimed in claim 4 or 5, wherein: the nano TiC particles and K2TiF6、KBF4、KCl、BaCl2The mass ratio of the mixed salt is 1: 7-1: 10.
8. The method for preparing the aluminum master alloy containing the multi-scale mixed particles as recited in claim 5, wherein: and in the step 6, the aluminum melt is uniformly stirred in an electromagnetic stirring mode.
9. The method for preparing the aluminum master alloy containing the multi-scale mixed particles as recited in claim 5, wherein: and 6, uniformly stirring the aluminum melt by adopting an electrically controlled mechanical stirring mode with a propeller type stirring head, wherein the rotating speed of the stirring head is 150-250 rmp/min.
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