CN113322392A - Preparation method of nano silicon carbide particle reinforced aluminum alloy matrix composite material - Google Patents
Preparation method of nano silicon carbide particle reinforced aluminum alloy matrix composite material Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
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- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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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
- C22C32/0052—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 carbides
- C22C32/0063—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 carbides based on SiC
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- 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
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22F1/047—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 magnesium as the next major constituent
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- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
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Abstract
The invention relates to the field of metal matrix composite preparation, and particularly discloses a preparation method of a nano silicon carbide particle reinforced aluminum alloy matrix composite. And (3) clamping the nano silicon carbide particles, the alloy element powder or the thin sheet between a plurality of aluminum plates, rolling at room temperature, folding in half along the rolling direction after rolling, and repeating the rolling-folding process for a plurality of times. And repeatedly heating and rolling the rolled sample to obtain the final completely densified bulk aluminum alloy base composite material. In the multi-pass rolling process, under the action of severe plastic deformation, the alloy elements are gradually dissolved into the aluminum matrix to achieve the effect of solid alloying, and the aluminum alloy matrix is formed; and silicon carbide particles are uniformly dispersed in the aluminum alloy matrix. The equipment required by the method is an industrial rolling mill and a muffle furnace, the process is simple, all elements in the obtained composite material are dissolved in solid solution, the nano particles are uniformly dispersed, the crystal grains are fine, and the strength and the toughness are excellent.
Description
Technical Field
The invention relates to a preparation method of a nano silicon carbide particle reinforced aluminum alloy matrix composite material, belonging to the field of composite material preparation.
Background
The aluminum-based composite material is a material formed by compounding aluminum or an aluminum alloy as a matrix and fibers, whiskers or particles as a reinforcement. It can obtain the advantages of good toughness of aluminium matrix and high strength of ceramic granules, and is a structural material with excellent comprehensive performance. In addition, the aluminum matrix composite material also has the advantages of high specific strength, small thermal expansion coefficient, good electric and heat conducting properties and the like, and is widely applied to the fields of aerospace, transportation and the like. The aluminum-based composite materials may be classified into pure aluminum-based composite materials and aluminum alloy-based composite materials according to the type of the matrix. Because the aluminum alloy has higher strength, the aluminum alloy matrix composite has higher strength than the pure aluminum matrix composite. Therefore, an aluminum alloy-based composite material is a preferred material in which high specific strength is sought.
The reinforcement particles can be divided into nanoparticles and microparticles. Compared with the micro-particles, the nano-particles have better strengthening effect on the aluminum matrix, and can increase more strength under the same content. Thus, reinforcing an aluminum alloy-based composite material using nanoparticles may have higher tensile strength.
The difficulty of the nano-particle reinforced aluminum alloy matrix composite material lies in the preparation process thereof. The preparation process of the composite material mainly comprises a liquid method and a solid method, and comprises casting, 3D printing, friction stir welding, powder metallurgy and the like. Certain metallurgical defects exist in the solidification process of the liquid method, and the performance of the material is reduced. In addition, the liquid process also has the problem of agglomeration of nanoparticles. Agglomeration of the nanoparticles can substantially reduce the strengthening effect of the nanoparticles and can even lead to brittle failure of the material. In the powder metallurgy of the solid-state method, the nanoparticles cannot penetrate into the powder, and cannot be uniformly dispersed in the aluminum alloy matrix. Therefore, the nanoparticles cannot be uniformly dispersed in either the solid-state method or the liquid-state method, and thus an aluminum alloy-based composite material having excellent properties cannot be prepared. Meanwhile, the conventional way to prepare the aluminum alloy-based composite material is to use aluminum alloy as a raw material. That is, it is required to prepare an aluminum alloy matrix first and then add a reinforcing phase to the aluminum alloy matrix. Obviously, the traditional preparation process needs more process links and higher cost. Therefore, it is necessary to develop a preparation process which is simple in process and excellent in performance of the prepared composite material.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a nano silicon carbide particle reinforced aluminum alloy matrix composite material. According to the method, the alloy elements and the nano silicon carbide particles with corresponding mass are added into the solid aluminum sheet, the alloy elements and the nano particles are subjected to solid solution and uniform distribution in the matrix through deformation of multi-pass rolling, the uniformity and the density of the material are further improved through high-temperature rolling, and the prepared aluminum alloy matrix is completely subjected to solid solution of the alloy elements and uniform distribution of the nano particles and has excellent strength and toughness. The method only needs an industrial rolling mill and a muffle furnace, and is suitable for large-scale industrial application.
The technical scheme provided by the invention is as follows:
a preparation method of a nano silicon carbide particle reinforced aluminum alloy matrix composite material comprises the following steps:
(1) placing alloy element powder and nano silicon carbide particles in a volatile organic solvent to be mixed into uniform suspension;
(2) taking an aluminum sheet substrate with uniform thickness, uniformly coating the turbid liquid obtained in the step (1) on the surface of an aluminum sheet, and stacking a plurality of aluminum sheets coated with the turbid liquid together after the organic solvent is completely volatilized to obtain a laminated blank;
(3) performing multi-pass room temperature rolling on the laminated blank obtained in the step (2), folding the laminated blank in half along the rolling direction after each pass of rolling, then performing rolling, and repeating the folding-rolling step for multiple passes (preferably, the number of repeated passes is more than or equal to 50, and most preferably, 70) to obtain an intermediate material;
(4) placing the intermediate material obtained in the step (3) in a muffle furnace at 300-600 ℃ for heat preservation for 3-30 minutes (preferably in the muffle furnace at 400-500 ℃ for heat preservation for 3-5 minutes), immediately taking out the intermediate material for hot rolling and thinning, repeating the heat preservation-rolling step to ensure that the accumulated thickness direction reduction is more than 70% (preferably repeating 2-5 times), and immediately performing quenching treatment after the last rolling;
(5) and (3) performing aging treatment on the material quenched in the step (4) as required to obtain the nano silicon carbide particle reinforced aluminum alloy matrix composite, wherein the aging treatment is not required when a non-aging reinforced aluminum alloy matrix is prepared, and the nano silicon carbide particle reinforced aluminum alloy matrix composite is obtained after the quenching treatment in the step (4).
Preferably, the alloying element in step (1) is at least one of common aluminum alloying elements, such as: magnesium, copper, zinc, and the like.
Preferably, the alloying elements in step (1) may also be a sheet-like material, which is not mixed with silicon carbide particles but added in step (2) by alternately stacking with aluminum sheets.
Preferably, the mass ratio of the alloying element powder in step (1) to the aluminum sheet matrix in step (2) is 1% to 20% (more preferably 4.5% to 10%).
Preferably, the volatile organic solvent in step (1) is absolute ethanol.
Preferably, the mass ratio of the nano silicon carbide particles in the step (1) to the aluminum sheet matrix in the step (2) is 3 to 20% (more preferably 6 to 12%).
Preferably, the diameter of the nano silicon carbide particles in the step (1) is 10-500 nm.
Preferably, the aluminum sheet matrix in step (2) is a pure aluminum sheet.
Preferably, step (3) wraps the laminated blank of step (2) in a steel sheet before room temperature rolling, and then room temperature rolling is performed.
Preferably, in the multi-pass room temperature rolling process in the step (3), the reduction of the thickness of the rolled sample in each pass is more than or equal to 50%.
Preferably, the room temperature rolling in the step (3) can be replaced by forging or extrusion deformation.
Preferably, the temperature and time of the aging treatment in the step (5) are carried out according to a conventional aging treatment mode according to the added alloy elements.
In the technical scheme of the invention, other industrial alloy materials can be prepared by replacing the aluminum sheet substrate with other metal materials such as copper sheets or copper alloy sheets.
The principle of the invention mainly comprises: and (3) clamping the nano silicon carbide particles and the alloy powder between a plurality of aluminum plates, rolling at room temperature, folding in half along the rolling direction after rolling, and repeating the rolling-folding process for a plurality of times. And heating and high-temperature rolling the rolled sample, and repeating the steps for a plurality of times to obtain the finally densified bulk material. During the rolling process at room temperature, under the action of severe plastic deformation, the alloy particles and the silicon carbide particles are gradually and uniformly dispersed. Meanwhile, the alloy particles are crushed by concentrated stress and gradually refined to a nano-scale. Dislocation channels generated by deformation and local temperature rise accelerate diffusion of alloy elements to make the alloy elements solid-dissolved. High-temperature rolling further dissolves alloy elements, and densification and defects are reduced. The equipment required by the method is an industrial rolling mill and a muffle furnace, the process is simple, all elements in the prepared composite material are dissolved in solid solution, the nano particles are uniformly dispersed, the crystal grains are fine, and the strength and the toughness are excellent.
Compared with the prior art, the invention has the beneficial effects that:
1. the method only needs multi-pass rolling and hot rolling treatment, and the equipment is an industrial rolling mill and a muffle furnace, so that industrial large-scale production can be realized.
2. The invention directly adopts pure aluminum and alloy element powder to prepare the aluminum alloy matrix composite material, does not need an aluminum alloy material as an initial material, and reduces the process links and the cost.
3. The nano particles in the aluminum alloy matrix composite material prepared by the method are uniformly dispersed, and the aluminum alloy matrix composite material is beneficial to strengthening of the aluminum alloy.
4. The aluminum alloy matrix composite material prepared by the invention has excellent toughness.
Drawings
FIG. 1 is a flow chart of the preparation process of the nano silicon carbide particle reinforced aluminum alloy matrix composite material.
FIG. 2 is a scanning electron microscope and elemental distribution diagram of the composite material prepared in example 1 of the present invention.
FIG. 3 is a scanning electron microscope and elemental distribution diagram of the composite material prepared in example 2 of the present invention.
FIG. 4 is a scanning electron microscope and elemental distribution plot of the composite material prepared in example 3 of the present invention.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
FIG. 1 is a flow chart of the preparation process of the nano silicon carbide particle reinforced aluminum alloy matrix composite material. In the following examples, when non-age strengthened aluminum alloys, such as Al-Mg alloys, are produced, no aging treatment is required.
Embodiment 1 a method for preparing a nano silicon carbide particle reinforced aluminum alloy matrix composite, comprising the steps of:
the composite material prepared in the embodiment takes Al-4.5 wt% of Mg alloy as a matrix, and SiC with the mass fraction of 10% as a reinforcement. Wherein the particle diameter of the SiC particles is 50 nm.
(1) Cutting a pure aluminum sheet with the size of 125 multiplied by 50 multiplied by 0.25mm, taking 8 sheets as an original matrix, and polishing and cleaning the surface of a sample;
(2) according to the mass of the aluminum sheet, magnesium powder accounting for 4.5 percent of the mass of the aluminum sheet and nano SiC particles accounting for 10 percent of the mass of the aluminum sheet are weighed. Placing the two kinds of particles in a beaker, pouring a proper amount of absolute ethyl alcohol into the beaker, and carrying out ultrasonic oscillation until the two kinds of particles are uniformly mixed to obtain a suspension.
(3) And (3) uniformly coating all the turbid liquid obtained in the step (2) on the surface of the aluminum sheet obtained in the step (2), and stacking 8 aluminum sheets coated with the turbid liquid together after the absolute ethyl alcohol is completely volatilized to obtain a laminated blank.
(4) And (4) wrapping the laminated blank obtained in the step (3) by using a steel plate, rolling at room temperature (25 ℃, the same below), folding the aluminum sheet in half along the rolling direction after each pass of rolling, wrapping by using the steel plate, and rolling. And then, the folding-rolling steps are repeated to required passes, the rolling is carried out for 70 passes at room temperature in the embodiment, and the reduction of the thickness of the sample after each pass of rolling is more than or equal to 50 percent, so that the intermediate material is obtained.
(5) High-temperature densification: carrying out high-temperature rolling treatment on the intermediate material obtained in the step (4): and (3) putting the intermediate material into a 400 ℃ muffle furnace for heat preservation for 3 minutes, immediately taking out the intermediate material after the heat preservation time is up, performing hot rolling and thinning, then putting the intermediate material into the 400 ℃ muffle furnace for heat preservation for 3 minutes, repeating the heat preservation-rolling steps for 4 times, and accumulating the rolling reduction in the thickness direction to be more than 70%. And immediately putting the rolled steel into water for quenching after the last pass of rolling is finished, and ensuring that the cooling speed reaches more than 400K/s to obtain the final Al-Mg/SiC composite material.
Fig. 2(a) - (b) are scanning electron microscope pictures of the final sample in this example 1, and it can be seen that the dispersibility of the nanoparticles is very good. Fig. 2(c) - (f) are scanning electron microscope element distribution diagrams of the composite material prepared in this example 1, and it can be seen that the alloying elements are all uniformly dispersed in the aluminum matrix, indicating that the alloying elements are all dissolved in the aluminum matrix.
The composite material prepared by the method of the embodiment has tensile strength as high as 580MPa, elongation at break of 7 percent and excellent toughness.
Example 2
The composite material prepared in this example uses an Al-10 wt% Mg alloy as a matrix and 6 wt% SiC as a reinforcement. Wherein the particle diameter of the SiC particles is 50 nm.
(1) Pure aluminum sheets of 125X 50X 0.25mm size were cut, 8 sheets were taken as the original substrate, and the surface of the sample was ground and cleaned.
(2) According to the mass of the aluminum sheet, 10% of magnesium powder and 6% of nano SiC particles are weighed. Both granules were placed in a beaker (or similar container), poured into the appropriate amount of absolute ethanol and shaken ultrasonically. And obtaining turbid liquid with two kinds of particles uniformly mixed through ultrasonic oscillation. And (3) uniformly coating the suspension on the surface of the aluminum sheet obtained in the step (1), and stacking a plurality of aluminum sheets coated with the suspension together after the absolute ethyl alcohol is completely volatilized to obtain a laminated blank.
(3) And (3) wrapping the laminated blank obtained in the step (2) in a steel sheet for rolling deformation, folding the aluminum sheet in half along the rolling direction after each pass of rolling, and then rolling. And (4) repeatedly folding and rolling until the required pass is reached, wherein the pass is more than or equal to 70, and the reduction of the thickness of the sample rolled in each pass is more than or equal to 50%, so as to obtain the intermediate material.
(4) And (4) placing the intermediate material obtained in the step (3) in a 400 ℃ muffle furnace for heat preservation for 3 minutes, immediately taking out the intermediate material for hot rolling and thinning, and repeating the heat preservation-rolling cycle for 3 times, wherein the accumulated thickness direction reduction is more than 70%. And immediately quenching after the last pass of rolling is finished, and ensuring that the cooling speed reaches more than 400K/s to obtain the final Al-Mg/SiC composite material.
Fig. 3(a) - (b) are scanning electron microscope pictures of the final sample in this example 2, and it can be seen that the dispersibility of the nanoparticles is very good. FIGS. 3(c) - (f) are SEM element distribution diagrams of the composite material prepared in this example 2, and it can be seen that the alloying elements are all uniformly dispersed in the aluminum matrix, indicating that the alloying elements are all dissolved in the aluminum matrix.
The tensile strength of the composite material prepared by the method of the embodiment is as high as 430MPa, the elongation at break is 4%, and the composite material has good mechanical properties.
Example 3
The composite material prepared in this example uses an alloy of Al-5.6% Zn-2.5% Mg-1.5Cu (wt%) as a matrix and 12 wt% SiC as a reinforcement. Wherein the particle diameter of the SiC particles is 50 nm.
(1) Pure aluminum sheets of 125X 50X 0.25mm size were cut, 8 sheets were taken as the original substrate, and the surface of the sample was ground and cleaned.
(2) According to the mass of the aluminum sheet, 5.6 percent, 2.5 percent and 1.5 percent of zinc powder, magnesium powder, copper sheet and 12 percent of nano SiC particles are weighed respectively. These powders were placed in a beaker (or similar container), poured into a suitable amount of anhydrous ethanol and sonicated. Obtaining turbid liquid with uniformly mixed particles through ultrasonic oscillation, uniformly coating the turbid liquid on the surface of the aluminum sheet obtained in the step (1), directly placing a copper sheet on the surface of the aluminum sheet after the absolute ethyl alcohol is completely volatilized, and stacking a plurality of aluminum sheets coated with the turbid liquid and provided with the copper sheets together to obtain a lamination blank.
(3) And (3) wrapping the laminated blank obtained in the step (2) in a steel sheet for rolling deformation, folding the aluminum sheet in half along the rolling direction after each pass of rolling, and then rolling. And (4) repeatedly folding and rolling until the required pass is reached, wherein the pass is more than or equal to 70, and the reduction of the thickness of the sample rolled in each pass is more than or equal to 50%, so as to obtain the intermediate material.
(4) And (4) placing the intermediate material obtained in the step (3) in a muffle furnace at 500 ℃ for heat preservation for 5 minutes, immediately taking out the intermediate material for hot rolling and thinning, and repeating the heat preservation-rolling cycle for 3 times, wherein the accumulated thickness direction reduction is more than 70%. And immediately quenching after the last pass of rolling is finished, and ensuring that the cooling speed reaches more than 400K/s to obtain the solid-solution aluminum alloy matrix composite.
(5) And (4) preserving the solid-solution aluminum alloy matrix composite material obtained in the step (4) in a muffle furnace at the temperature of 120 ℃ for 12 hours for aging treatment, and obtaining the final Al-Zn-Mg-Cu/SiC composite material after the treatment is finished.
Fig. 4(a) - (b) are scanning electron microscope pictures of the final sample in this example 3, and it can be seen that the dispersibility of the nanoparticles is very good. Fig. 4(c) - (h) are the pictures of the distribution of the elements by sem of the final sample in this example 3, and it can be seen that the alloying elements are all uniformly dispersed in the aluminum matrix, indicating that the alloying elements are all dissolved in the aluminum matrix.
The tensile strength of the composite material prepared by the method of the embodiment is up to 650MPa, the elongation at break is 8.5%, and the composite material has excellent toughness.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (9)
1. The preparation method of the nano silicon carbide particle reinforced aluminum alloy matrix composite is characterized by comprising the following steps of:
(1) placing alloy element powder and nano silicon carbide particles in a volatile organic solvent to be mixed into uniform suspension;
(2) taking an aluminum sheet substrate with uniform thickness, uniformly coating the turbid liquid obtained in the step (1) on the surface of an aluminum sheet, and stacking a plurality of aluminum sheets coated with the turbid liquid together after the organic solvent is completely volatilized to obtain a laminated blank;
(3) performing multi-pass room temperature rolling on the laminated blank obtained in the step (2), folding the laminated blank in half along the rolling direction after each pass of rolling, then performing rolling, and repeating the folding-rolling step for multiple passes to obtain an intermediate material;
(4) placing the intermediate material obtained in the step (3) in a muffle furnace at 300-600 ℃ for heat preservation for 3-30 minutes, immediately taking out the intermediate material for hot rolling, repeating the heat preservation-rolling step to ensure that the accumulated thickness direction reduction is more than 70%, and immediately performing quenching treatment after the last pass of rolling is finished;
(5) and (3) performing aging treatment on the material quenched in the step (4) as required to obtain the nano silicon carbide particle reinforced aluminum alloy matrix composite, wherein the aging treatment is not required when a non-aging reinforced aluminum alloy matrix is prepared, and the nano silicon carbide particle reinforced aluminum alloy matrix composite is obtained after the quenching treatment in the step (4).
2. The method according to claim 1, wherein the alloying element in the step (1) is at least one of magnesium, copper and zinc.
3. The method according to claim 1, wherein the alloying elements in step (1) are also in the form of a sheet-like material, and are not mixed with silicon carbide particles, but are added in step (2) by alternately stacking aluminum sheets.
4. The preparation method according to claim 1, wherein the mass ratio of the alloying element in the step (1) to the aluminum sheet substrate in the step (2) is 1-20%.
5. The method according to claim 1, wherein the diameter of the nano silicon carbide particles in step (1) is 10 to 500 nm.
6. The preparation method according to claim 1, wherein the mass ratio of the nano silicon carbide particles in the step (1) to the aluminum sheet matrix in the step (2) is 3-20%.
7. The preparation method according to claim 1, wherein in the step (3), in the process of carrying out the multi-pass room temperature rolling, the reduction of the thickness of the rolled sample in each pass is equal to or more than 50%, and the pass of the room temperature rolling is equal to or more than 50%.
8. The method according to claim 7, wherein the step (3) comprises wrapping the laminated blank of the step (2) in a steel sheet before rolling at room temperature, and then rolling.
9. The method according to claim 1, wherein the room temperature rolling in step (3) is replaced by forging or extrusion.
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