CN114351000B - Preparation method of in-situ nano-particle and rare earth coupling reinforced aluminum-based composite material - Google Patents
Preparation method of in-situ nano-particle and rare earth coupling reinforced aluminum-based composite material Download PDFInfo
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- CN114351000B CN114351000B CN202111559921.8A CN202111559921A CN114351000B CN 114351000 B CN114351000 B CN 114351000B CN 202111559921 A CN202111559921 A CN 202111559921A CN 114351000 B CN114351000 B CN 114351000B
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Abstract
The invention relates to an in-situ nano-particle and rare earth coupling reinforced aluminum-based composite material and a preparation method thereof. And applying an acoustic-magnetic coupling field in the reaction process to obtain the composite material of the uniformly distributed nano enhanced phase clusters and the fine crystalline structures. And then, by means of an optimized hot extrusion technology and a three-stage aging treatment technology, the defects of the material are reduced, the dynamic recrystallization of the subgrain in the material is promoted, fine recrystallized grains are obtained, the strength, the plasticity, the impact resistance and the corrosion resistance of the material are improved, the comprehensive performance of the material is improved to the greatest extent, and the qualified aluminum-based composite material section for the railway train body is obtained.
Description
Technical Field
The invention relates to an aluminum-based composite material, in particular to a preparation method of in-situ nano particles and mixed rare earth reinforced aluminum alloy for a light rail train body.
Background
The light weight of the rail transit equipment is a necessary way for upgrading the modern high-speed train, and the weight reduction has important practical significance on aspects of vehicle speed increase, noise reduction, energy conservation and the like. The metal structure material used for the light weight of the traffic equipment firstly pushes aluminum alloy and magnesium alloy, in particular aluminum alloy. At present, the high-speed train bodies of various countries basically adopt aluminum alloy frameworks. In addition, many parts such as a body cover and a gear box body are also made of aluminum. For the rail vehicle, the weight of the vehicle body structure accounts for 15% -30% of the weight of the whole vehicle, so that the weight reduction of the vehicle body is significant for accelerating rail traffic. At present, the aluminum alloy for rail transit vehicle bodies is mainly 6N01,7N01 and 7003 section bars.
With the increasing energy crisis, environmental pollution and safety problems in the world traffic field, the light weight and high performance of key structural components of rail traffic have become important development directions and inevitable trends. Meanwhile, with the influence of environmental pollution and climate deterioration, vehicles are increasingly in contact with corrosive media, and it becomes equally important to improve the corrosion resistance of aluminum alloys. Chinese patent 201910221572.5 discloses a high-performance easily welded rail train body and a manufacturing method thereof, wherein independent door corners of the body are all made of in-situ nano ceramic particle reinforced aluminum matrix composite materials, and an extruded material for a rail train is obtained. In recent years, the preparation technology of the in-situ nano ceramic particle reinforced aluminum matrix composite material has made breakthrough development. The invention patent of the Chinese patent 201711114899.X breaks through the inversion relation of strong plasticity through the actions of Orowan strengthening, fine grain strengthening, nano reinforcement toughening, nano precipitated phase dispersion strengthening, damping effect of nano precipitated phase and the thinning and modification effect of rare earth, and obtains the extrudable aluminum-based composite material with strong plasticity, impact resistance and fatigue resistance.
According to the prior art and patents, the mechanical property of the aluminum alloy is almost improved simply by microalloying or introducing a proper amount of nano particles into the aluminum alloy. The bottleneck problems that the material performance is improved to a limited extent and high strength, high toughness and corrosion resistance are difficult to be considered exist only by depending on rare earth microalloying. The in-situ nano-particle reinforced aluminum alloy is prepared by taking appropriate gas-phase, liquid-phase or powder-phase solid phase as a reactant and carrying out chemical reaction on the reactant and a matrix melt under a certain reaction temperature condition, overcomes the problem that the strength-plasticity (or toughness) of the conventional micron-sized particle reinforced aluminum-based composite material is in an inverted relation, and has higher strength, toughness, corrosion resistance, fatigue resistance and weldability. However, the clustering problem of the nanoparticles has been a difficult point in the research of particle recombination, so that the materials are easy to corrode at the interface. Therefore, a novel rail train body material with light weight, high strength, high toughness and corrosion resistance is urgently needed to be developed.
Disclosure of Invention
The invention aims to develop a preparation method of an aluminum alloy for a light rail train body by utilizing the coupling effect of in-situ nanoparticles and mixed rare earth aiming at the defects of the prior art, and the obdurability and corrosion resistance of the rail train body are obviously improved.
The second purpose of the invention is to improve the comprehensive performance of the aluminum alloy by regulating and controlling the content and distribution of the nanoscale reinforcing phase in the composite material. The strengthening effect of the rare earth-containing precipitated phase strengthening phase on the matrix alloy has a peak value no matter the nanometer in-situ nanometer particle strengthening phase or the rare earth-containing precipitated phase strengthening phase finally generated by adding the mixed rare earth. The in-situ nano-particles and the rare earth precipitated phase belong to two strengthening phases with different properties, and the combination of the strengthening phases and the rare earth precipitated phase does not conflict. The novel aluminum-based composite material has the advantages that the tensile strength, the elongation and the corrosion resistance are further improved macroscopically.
An in-situ nano reinforced rare earth aluminum alloy for a light rail train body comprises the following aluminum alloy matrix components in percentage by mass: 4-5% of Zn, 1-2% of Mg, less than 0.2% of Cu, 0.2-0.7% of Mn, less than 0.3% of Cr, 0.2% of Ti woven fabrics and the balance of Al.
The preparation method comprises the following steps:
melting an aluminum alloy matrix at 760-790 ℃, preserving heat for 10-15min, then heating the melt to 840-870 ℃, pressing dried reaction powder wrapped by high-purity aluminum foil into the melt through a high-purity graphite bell jar, applying an acousto-magnetic coupling field, reacting for 20-40min, and refining and slagging off after the reaction is finished; reducing the temperature to 720-760 ℃, adding the mixed rare earth into the melt, simultaneously applying an acoustic-magnetic coupling field, reacting for 20-40min, refining and slagging off, and pouring into a copper mold to obtain a composite material cast rod; and then carrying out hot extrusion deformation processing and subsequent heat treatment on the aluminum alloy cast rod to finally obtain the in-situ nano reinforced rare earth aluminum alloy extrusion piece for the railway train body.
The reaction powder coated by the high-purity aluminum foil is potassium fluozirconate (K) 2 ZrF 6 ) Potassium fluoroborate (KBF) 4 ) Reacting to generate in-situ nano ZrB 2 Particles, zrB 2 The particle size is 50-100nm, potassium fluorozirconate (K) 2 ZrF 6 ) And potassium fluoroborate (KBF) 4 ) In a molar ratio of 19:46, zrB of 1-3 percent of the mass of the aluminum alloy matrix can be obtained 2 . Adding the mixed rare earth by adopting a mode of Al-20wt.% RE intermediate alloy, and generating nano Al after aging 3 Sc particles, nano Al 3 The size of Sc particles is 30-60nmThe addition amount of the mixed rare earth is 0.1-0.7% of the mass of the aluminum alloy matrix.
The mixed rare earth comprises the following components in percentage by weight: scandium content 65wt.%, erbium content 15wt.%, lanthanum content 8wt.%, praseodymium content 7wt.%, neodymium content 5wt.%.
The preparation method of the mixed rare earth intermediate alloy comprises the following steps: preheating a graphite crucible, adding an aluminum block, heating to 720-750 ℃ until the aluminum block is fully melted into a liquid state, degassing and slagging off. In the preparation process of the intermediate alloy, the burning loss of aluminum is proportioned according to 1 percent, and the burning loss of rare earth is proportioned according to 10 percent. And then wrapping the mixed rare earth powder with aluminum foil, adding the wrapped mixed rare earth powder into a crucible, fully stirring the mixture, and keeping the temperature for 30min. And then carrying out high-energy intermittent ultrasonic treatment on the alloy melt, setting the ultrasonic frequency to be 1.5KHz, and extending the preheated ultrasonic energy concentrator into a position which is 10-20 mm away from the surface of the alloy melt. And (3) carrying out ultrasonic treatment for 15min, reheating the melt to 730 ℃, carrying out ultrasonic treatment for 15min again, degassing and deslagging, and then casting and cooling by using a preheated mold to obtain the mixed rare earth master alloy Al-20wt.% RE.
The external field in the reaction process is assisted by an acoustic-magnetic coupling field, namely a low-frequency magnetic field and a high-energy ultrasonic field. A low-frequency magnetic field with the frequency of 5-15Hz and the magnetic current of 60-120A; a high-energy ultrasonic field with the power of 900-1300W and the frequency of 15-25kHz; the application of the acoustic-magnetic coupling field in the reaction process can promote the reaction, improve the yield of the particles, improve the wettability of the particles and the matrix, uniformly distribute the particles in the matrix, ensure the uniform concentration of each area in the melt, inhibit the growth of the particles and refine the particles. In addition, the phenomenon that particles are deviated and gathered outside due to a single magnetic field and cavitation bubbles are distributed along the axial direction of the amplitude transformer due to single ultrasonic long acoustic flow motion can be avoided, and the defect of a single physical field is overcome.
The hot extrusion deformation processing technology comprises the following steps: and processing the homogenized cast ingot into a bar material for extrusion according to the required size, feeding the bar material into a resistance furnace, heating to 460-500 ℃, preserving heat for 0.8-1.2h, then heating an extrusion die to 410-460 ℃, preserving heat for 10-30min, and carrying out hot extrusion at the extrusion speed of 2-5 mm/s.
The heat treatment is an optimized three-stage aging heat treatment process, and solid solution is carried out: and (3) water quenching at the temperature of 460-480 ℃ and the heat preservation time of 1-2 h. Artificial aging: the temperature is 100-120 ℃, the heat preservation time is 9-11h, the temperature is 130-150 ℃, and the heat preservation time is 7-9h.
The invention has the beneficial effects that:
the invention provides a preparation method of lightweight in-situ nano-particles and a mixed rare earth reinforced aluminum-based composite material, which obtains in-situ nano ZrB by combining the regulation and control of an in-situ direct melt reaction technology and an acoustic-magnetic coupling field technology 2 Particles (50-100 nm) and nano Al 3 Sc particles (30-60 nm) are uniformly distributed and have fine grains, and the in-situ reinforced rare earth aluminum alloy material is cast. Through a hot extrusion deformation process and three-stage aging heat treatment, the composite material prepared by the method has high strong plasticity and impact resistance, and the nano-particle ZrB prepared by the method has high strength, plasticity and impact resistance 2 Particles and rare earth strengthening phase Al 3 Sc can effectively improve the corrosion resistance of the material. The application can improve the strength and the rigidity of the train body when being applied to the train body of the rail train, and is related to the safe reliability and the comfort of the operation. The corrosion resistance and corrosion resistance of the vehicle body and the surface protection are related to the appearance, service life and maintenance system of the vehicle.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings which are needed to be used will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic view of an apparatus of the present invention;
1. a load coil 2, an electromagnetic stirring device 3, an aluminum alloy melt 4, a crucible 5 and a high-energy ultrasonic device.
FIG. 2 is a flow chart of the preparation process of the present invention
FIG. 3 is a structural drawing of an organization of in-situ nanoparticles and misch metal reinforced aluminum alloy for a railcar body according to the present invention; wherein the in-situ nanoparticles are 3% of the mass of the aluminum alloy matrix left unchanged, (a) 0wt.% RE (b) 0.1wt.% RE (c) 0.2wt.% RE; (d) 0.3wt.% RE.
FIG. 4 shows ZrB in the in-situ nanoparticles and the misch metal reinforced aluminum alloy for a railway train body according to the invention 2 Morphology of the particles.
FIG. 5 shows in-situ nanoparticles and mixed rare earth reinforced Al alloy for railborne train bodies according to the present invention 3 And (3) a morphology graph of the Sc mixed rare earth strengthening phase.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments which can be obtained by those skilled in the art based on the embodiments of the present invention without any creative work belong to the protection scope of the present invention.
Example 1:
(1) Aluminum alloy casting: melting 1Kg of aluminum alloy raw material at 790 ℃, preserving heat for 10min, then raising the temperature of the melt to 850 ℃, adding the dried reaction powder (the granularity is less than 100 mu m, the mass of potassium fluozirconate is 74g, and the mass of potassium fluoborate is 80 g) wrapped by high-purity aluminum foil into the melt in batches, simultaneously starting a combined device of a low-frequency magnetic field and a high-energy ultrasonic field (the magnetic field is 10Hz, the magnetic current is 100A; the ultrasonic is 900W, and the frequency is 20 kHz), reacting for 30min, removing scum on the surface of the melt after the reaction is finished, spraying hexachloroethane into the solution for refining, pouring the solution into a copper mold, and obtaining 3wt.% of ZrB 2 An aluminum matrix composite cast rod.
(2) Homogenization treatment: and (4) performing head cutting, tail cutting and face milling on the cast rod obtained in the step (1) to obtain a cast rod with the length of 200 mm. Then the cast rod is put into a box-type resistance furnace to be heated to 560 ℃ and kept for 24h.
(3) Hot extrusion treatment: and processing the homogenized cast ingot into an extrusion ingot blank according to the required size, feeding the extrusion ingot blank into a resistance furnace, heating to 460 ℃, preserving heat for 1.2h, then heating an extrusion die to 450 ℃, preserving heat for 20min, and carrying out hot extrusion at the extrusion speed of 2mm/s to obtain an extrusion bar with the diameter of 20 mm.
(4) Three-stage aging heat treatment: and (4) carrying out heat treatment on the extruded bar obtained in the step (3). Solid solution: the temperature is 480 ℃, and the heat preservation time is 1h. The quenching adopts water quenching. Artificial aging: the temperature is 110 ℃, and the heat preservation time is 10h; the temperature is 140 ℃, and the holding time is 8h. Finally obtaining the qualified in-situ particle reinforced rare earth aluminum alloy extrusion piece for the railway train body.
Example 2:
the preparation method is basically the same as that in example 1, except that: the reaction products are different, 145g of Al-20wt.% RE master alloy is added only at 750 ℃, and the acousto-magnetic coupling field is applied for reaction for 30min to obtain 0.2wt.% RE material cast rod.
Example 3:
the preparation method is basically the same as that in example 1, except that: the reactants with different mass are added with dried reaction powder (the granularity is less than 100 mu m, the mass of potassium fluozirconate is 74g, and the mass of potassium fluoborate is 80 g) wrapped by high-purity aluminum foil at 850 ℃, an acousto-magnetic coupling field is applied for reaction for 30min, scum on the surface of a melt is removed after the reaction is finished, hexachloroethane is sprayed into a solution for refining, 145g of Al-10wt.% RE intermediate alloy is added when the temperature is reduced to 750 ℃, and the ZrB with the weight percent of 3 is prepared by applying the acousto-magnetic coupling field for reaction for 30min (3 wt.% ZrB) 2 +0.2wt.% RE) aluminum matrix composite cast bars.
Each example is a composite of in situ nanoparticles with different volume fractions, and the specific mechanical properties are shown in the following table:
table 1 shows the results of testing the properties of the extruded materials of the nano-reinforced composite materials
Table 2 shows the results of testing the corrosion properties of the extruded materials of the nano-reinforced composite materials
Experiments prove that the rail train body disclosed by the invention and the rail train body adopted in the traditional method have the following outstanding advantages and effects: the tensile strength, the yield strength and the elongation are greatly improved, and the deformation amount is 60-85% in a quasi-static crushing test, so that the sample has no obvious cracks. After adding mixed rare earth, nano ZrB 2 The agglomeration and growth of the particles are obviously reduced, and Al 3 The Sc particles can obviously improve the corrosion resistance of the material. Comparison of examples 2 and 3 gives a granulate of 3wt.% ZrB 2 The performance of +0.2wt.% RE is obviously improved, so that the performance index of the embodiment of the invention always shows more excellent performance than that of the matrix alloy, and all the performances can meet the material requirement of the rail train body.
The invention provides a preparation method of in-situ nano particles and mixed rare earth reinforced aluminum-based composite material for a light rail train body, which combines the precise control of the technological parameters of the preparation method and the selection of the volume fraction of the particles to obtain a light, high-strength, high-toughness and corrosion-resistant rail train body material, provides a reference basis for preparing high-performance rail train body materials in the future, and has wide market prospect and economic value.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. The preparation method of the in-situ nano-particle and rare earth coupling reinforced aluminum matrix composite is characterized by comprising the following specific steps: melting an aluminum alloy matrix at 760-790 deg.C, maintaining the temperature for 10-15min, heating the melt to 840-870 deg.C, pressing into dried reaction powder wrapped with high-purity aluminum foil through high-purity graphite bell jar, introducing into the melt, applying acousto-magnetic coupling field, and reacting for 20Refining and slagging-off treatment are carried out after the reaction is finished for-40 min; reducing the temperature to 720-760 ℃, adding the mixed rare earth into the melt, simultaneously applying an acoustic-magnetic coupling field, reacting for 20-40min, refining and slagging off, and pouring into a copper mold to obtain a composite material cast rod; carrying out hot extrusion deformation processing and subsequent heat treatment on the aluminum alloy cast rod to finally obtain an in-situ nano reinforced rare earth aluminum alloy extrusion piece for the railway train body; the aluminum alloy matrix comprises the following components in percentage by mass: zn 4-5%, mg 1-2%, cu<0.2%，Mn 0.2-0.7%，Cr <0.3, Ti <0.2, and the balance of Al; the reaction powder coated by the high-purity aluminum foil is potassium fluozirconate and potassium fluoborate, and in-situ nanometer ZrB is generated by reaction 2 Particles of ZrB 2 The particle sizes are all 50-100 nanometers, and the molar ratio of the potassium fluozirconate to the potassium fluoborate is 19:46, obtaining ZrB accounting for 1-3 percent of the mass of the aluminum alloy matrix 2 (ii) a The mixed rare earth is added by adopting a mode of Al-20 wt% RE intermediate alloy, and after aging, nano Al is generated 3 Sc particles, nano Al 3 The size of Sc particles is 30-60 nanometers, and the addition amount of the mixed rare earth is 0.1-0.7 percent of the mass of the aluminum alloy matrix; the mixed rare earth comprises the following components in percentage by weight: scandium content 65 wt%, erbium content 15 wt%, lanthanum content 8 wt%, praseodymium content 7 wt%, neodymium content 5 wt%; the acoustic magnetic coupling field is a low-frequency magnetic field and a high-energy ultrasonic field; a low-frequency magnetic field with the frequency of 5-15Hz and the magnetic current of 60-120A; a high-energy ultrasonic field with the power of 900-1300W and the frequency of 15-25kHz; the heat treatment is a three-stage aging heat treatment process, and solid solution is carried out: water quenching at 460-480 deg.C for 1-2 h; artificial aging: the temperature is 100-120 ℃, the heat preservation time is 9-11h, the temperature is 130-150 ℃, and the heat preservation time is 7-9h.
2. The method for preparing in-situ nano-particles and rare earth coupling reinforced aluminum matrix composite material according to claim 1, wherein the mixed rare earth intermediate alloy is prepared by the following method: preheating a graphite crucible, putting an aluminum block, heating to 720-750 ℃ until the aluminum block is fully melted into a liquid state, and then degassing and slagging off; in the preparation process of the intermediate alloy, the burning loss of aluminum is proportioned according to 1% and the burning loss of rare earth is proportioned according to 10%, then the mixed rare earth powder is wrapped by aluminum foil and added into a crucible, the crucible is fully stirred and is kept warm for 30min, then the alloy melt is subjected to high-energy intermittent ultrasonic treatment, the ultrasonic frequency is set to be 1.5kHz, a preheated ultrasonic energy concentrator extends into a position 10mm-20mm away from the surface of the aluminum alloy melt, ultrasonic treatment is carried out for 15min, the melt is reheated to 730 ℃, ultrasonic treatment is carried out for 15min again, and after degassing and deslagging, casting and cooling are carried out by using a preheated die, so that the mixed rare earth intermediate alloy Al-20wt.
3. The method for preparing in-situ nano-particle and rare earth coupling reinforced aluminum matrix composite material according to claim 1, wherein the hot extrusion deformation processing technology comprises: and processing the homogenized cast ingot into a bar material for extrusion according to the required size, feeding the bar material into a resistance furnace, heating to 460-500 ℃, preserving heat for 0.8-1.2h, then heating an extrusion die to 410-460 ℃, preserving heat for 10-30min, and carrying out hot extrusion at the extrusion speed of 2-5 mm/s.
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