CN111041288B - High-toughness anti-fatigue in-situ aluminum-based composite material and preparation method thereof - Google Patents
High-toughness anti-fatigue in-situ aluminum-based composite material and preparation method thereof Download PDFInfo
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- 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
- C22F1/057—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 copper as the next major constituent
Abstract
The invention relates to the field of in-situ nano-particle reinforced aluminum matrix composite materials, in particular to high-toughness anti-fatigue in-situ ZrB2A/AA 6111 aluminum matrix composite material and a preparation method thereof. The invention improves the obdurability and high cycle fatigue performance of the composite material simultaneously through dispersion strengthening and fine grain strengthening. In the preparation process, the reaction rate and the particle yield are improved by a multi-section electromagnetic control technology and an ultrasonic forming technology, and meanwhile, the particle agglomeration is reduced, so that the particle distribution is more uniform, more high-quality nucleation sites are formed, and the crystal grains are refined. In addition, by utilizing the synergistic effect of rare earth element Gd and an ultrasonic field, the ultrasonic field applied in the casting molding process purifies the surface of the ceramic particles, Gd atoms with larger atomic radius are easy to attach to the surface of the ceramic particles, the migration rate of a crystal boundary is reduced, crystal grains are refined, and meanwhile, the particle wettability is enhanced, so that the composite material has high strength and plasticity and high fatigue resistance.
Description
Technical Field
The invention relates to the field of in-situ nano-particle reinforced aluminum matrix composite materials, in particular to high-toughness anti-fatigue in-situ ZrB2A/AA 6111 aluminum matrix composite material and a preparation method thereof.
Background
In-situ nano ZrB2AA6111 aluminium baseThe composite material takes AA6111 as a matrix and ZrB2The ceramic particles are reinforcing phases, in-situ melt reaction is adopted in the preparation process to generate nano reinforcing particles, the particle size is nano, and the nano reinforcing particles have the characteristics of high strength, high specific modulus, wear resistance, impact resistance and the like; in the preparation process, the nano particles are easy to agglomerate and easily form a fatigue source under the action of cyclic load, so that the fatigue performance of the nano particles is reduced.
Chinese patent CN106702222A discloses a mixed rare earth doped (TiB)2+ZrB2) Method for producing a/Al composite material, in (TiB)2+ZrB2) Ce and Er elements are added on the basis of the/Al composite material, the obtained composite material has finer and more round crystal grains, and meanwhile, the mechanical property of the material is improved, but impurities exist in the interface of the particles and the matrix, so that the fatigue property of the material is reduced; chinese patent CN105220047A discloses a method for preparing a rare earth reinforced magnesium-aluminum-gadolinium-tin alloy plate, wherein Gd element is added on the basis of magnesium-aluminum alloy, and the strength is improved.
Chinese patent CN1676641A discloses a method for in-situ synthesis of magnetic chemical reaction for preparing metal-based nano composite material, which proposes in-situ synthesis of magnetic chemical reaction under a magnetic field steady magnetic field, an alternating magnetic field and a pulse magnetic field. Chinese patent CN101391290 discloses a method for preparing endogenetic particle reinforced metal matrix composite under the coupling action of magnetic field and ultrasonic wave, which utilizes the coupling action of magnetic field and ultrasonic wave to refine the particle size and disperse uniformly; the ultrasonic vibration stirring and electromagnetic stirring function improves the composite dynamic condition, and the particle phase and the matrix metal interface are better compounded.
However, the above patent still has the following problems: (1) impurities exist on the interface of the particles and the matrix, so that the wettability is reduced; (2) the particles are easy to gather at the periphery of the solution under the centrifugal action by electromagnetic stirring; (3) the application mode of the ultrasonic field is mainly that an ultrasonic probe is extended into the solution before casting, so that the probe is easy to corrode and introduce impurities, and the strength is not uniform enough; (4) the ultrasonic field cannot be applied during the cast molding process.
Disclosure of Invention
Aiming at the problems existing in the existing in-situ nano-particle reinforced aluminum-based composite material and the preparation process thereof, the invention provides a new improvement scheme, and in the preparation process, the particle distribution and the wettability of the particle and matrix interface are improved through the synergistic effect of rare earth element alloying, multi-section electromagnetic regulation and ultrasonic field regulation technologies, so that the toughness and the fatigue resistance of the in-situ nano ZrB2/AA6111 aluminum-based composite material are obviously improved.
The invention relates to high-toughness anti-fatigue in-situ ZrB2The preparation method of the AA6111 aluminum-based composite material improves the obdurability and the high-cycle fatigue performance of the composite material simultaneously through dispersion strengthening and fine grain strengthening. In the preparation process, the reaction rate and the particle yield are improved by a multi-section electromagnetic control technology and an ultrasonic forming technology, and meanwhile, the particle agglomeration is reduced, so that the particle distribution is more uniform, more high-quality nucleation sites are formed, and the crystal grains are refined. In addition, by utilizing the synergistic effect of rare earth element Gd and an ultrasonic field, the ultrasonic field applied in the casting molding process purifies the surface of the ceramic particles, Gd atoms with larger atomic radius are easy to attach to the surface of the ceramic particles, the migration rate of a crystal boundary is reduced, crystal grains are refined, and meanwhile, the particle wettability is enhanced, so that the composite material has high strength and plasticity and high fatigue resistance.
The technical scheme adopted by the invention comprises the following specific steps:
in the experiment, an Al-Zr-B system is adopted to prepare the particle-reinforced aluminum-based composite material, and the added reactant is mainly K2ZrF6And KBF4Powder, using 6111 aluminum alloy as a matrix. Firstly, respectively carrying out vacuum ball milling on two kinds of fluorine salts to 600-800 meshes, wherein the mass ratio of the ball materials is 5: 1-10: 1, the rotation speed is 200-300r/min, then the mixture is placed in a vacuum drying oven, the temperature is kept for 2-4h at 270 ℃ to remove crystal water, the required villiaumite is weighed according to a certain proportion after being dried according to the volume fraction of generated particles, the villiaumite is uniformly mixed and then is wrapped into small bags for standby by using aluminum foil paper, wherein the mass of each small bag is 15-30 g.Melting 6111 aluminum alloy, heating to 750 ℃ at 730-. After the reaction is finished, slagging off, refining and degassing are carried out, and the rare earth modified ZrB is obtained by pouring into an ultrasonic forming device shown in figure 1 when the temperature is reduced to 730-2A particulate reinforced aluminum matrix composite. The prepared material is subjected to hot extrusion deformation processing, and the tensile property and the fatigue property of the material are tested through a T6 heat treatment process.
The 6111 alloy comprises the following chemical components in percentage by mass: si: 0.6-1.1%, Mg: 0.5-1.1%, Cu: 0.5-0.9%, Fe <0.4%, Mn 0.1-0.45%, Zn: <0.15, the balance being Al.
The mass fraction of Gd in the Mg-Gd-added alloy is 87 percent, and the adding amount of Gd is 0.05 to 0.5 percent of the mass of AA 6111.
The KBF4And K2ZrF6The mass ratio of (A) to (B) is 1:1.08, and the reaction equation is as follows:
6KBF4+3K2ZrF6+10Al＝3ZrB2+K3AlF6+9KAlF4
the ZrB2The size of the particles is 50-90nm, the morphology of the particles is quadrilateral or hexagonal, ZrB2The volume fraction of the particles in the finally obtained ZrB2/AA6111 aluminum matrix composite is 1-3%.
The magnetic field applied by the electromagnetic regulation and control technology is a multi-section alternating magnetic field, so that the problem of centrifugal agglomeration of particles caused by a continuous directional magnetic field is solved, and the particles are distributed more uniformly. The frequency of the magnetic field is 8-17Hz, the intensity of the magnetic field is 0.03-0.09T, and the application mode of the magnetic field is as follows: stopping for 0.5-1min after applying the magnetic field for 4-6min, then applying the reverse magnetic field for 4-6min, and circulating in sequence until the reaction is finished. The aluminum melt generates induced current under the action of the magnetic field, the current and the magnetic field interact to generate electromagnetic force to drive the aluminum liquid to rotate, and the reaction salt and the generated ceramic particles are dispersed due to the impact force of the surrounding aluminum liquid because the conductivity and the permeability of the reaction salt and the ceramic particles are different from those of the surrounding aluminum liquid, so that the fluidity of the reaction salt and the contact area of the reaction salt and the aluminum liquid are increased, and the distribution of the ceramic particles in the aluminum liquid is more uniform; on the other hand, the magnetic field increases the reaction rate and conversion rate of the reaction by changing the orientation of the radicals and the time during which the radicals are present.
In the invention, ZrB2Rare earth Gd element accounting for 0.05-0.5 percent of matrix aluminum alloy is added into the particle reinforced 6111 aluminum matrix composite. The Gd element and Fe and Cu elements in the Al matrix form an intermediate compound, so that the aggregation of a net Fe-containing phase and a copper-rich phase is reduced, the length-diameter ratio of eutectic Si is reduced, and the continuity of the aluminum matrix is improved. In addition, in the solidification process, under the action of an ultrasonic field, the surface of the ceramic particle is purified, the Gd element with larger atomic radius is attached to the surface of the ceramic particle, the surface tension of the interface of the ceramic particle and an aluminum matrix is reduced, the wettability of the particle interface is improved, and the interface bonding condition of the particle and the matrix is improved.
The invention provides a device (as shown in figure 1) capable of casting and molding under an ultrasonic field, wherein a mold is placed into a cavity of the device before casting, the mold is in the ultrasonic field, the mold is preheated to 250 ℃ under the action of oil bath in the cavity of the device, the ultrasonic frequency applied during casting is 20000-. On one hand, the ultrasonic wave acts on the mixed melt to promote the wetting of the aluminum liquid on the ceramic particles, the surface of the ceramic particles is cleaned at high temperature and high pressure caused by the acoustic cavitation effect, the surface energy of the particle interface is reduced, and the bonding condition of the particle and the matrix interface is continuously adjusted in the solidification process of the molten liquid, so that the bonding condition of the particle and the matrix interface in the finally prepared material is obviously improved; on the other hand, the ultrasonic field effectively breaks up agglomerated particles, so that the distribution of the particles is more dispersed and the size of the particles is smaller; in addition, the ultrasonic field also reduces the porosity of the material, so that the prepared material has more uniform tissue.
Carrying out hot extrusion deformation processing on the prepared material, wherein the hot extrusion process comprises the following steps: the extrusion temperature is 440-500 ℃, the extrusion ratio is 16: 1, extruding at the speed of 3-5m/min, and water-cooling the extruded sample. Then carrying out T6 heat treatment on the alloy, wherein the process parameters are as follows: the solid solution temperature is 500-530 ℃, the solid solution time is 3-12h, the pre-aging is carried out at 80-100 ℃ for 20-30min after the solid solution treatment, then the aging is carried out at 170-185 ℃, the aging time is 1-5h, and the water cooling is carried out to the normal temperature after the aging is finished. The tensile and fatigue properties were then tested.
The invention provides a high-toughness anti-fatigue in-situ ZrB2The preparation method of the/AA 6111 aluminum-based composite material obtains the in-situ nano ZrB with uniform distribution of in-situ nano particles, fine crystal grains, good combination of the particles and a matrix interface and fine short rod-shaped eutectic Si phase by a rare earth modification and refinement technology, an electromagnetic regulation and control technology and an ultrasonic purification and forming technology2The performance of the AA6111 aluminum-based composite material reaches that the tensile strength is more than or equal to 378MPa, the yield strength is more than or equal to 309MPa, the elongation is more than or equal to 27 percent, and the fatigue strength is more than or equal to 115MPa, so that the composite material prepared by the invention has high strength and toughness and high fatigue resistance, and has wide application prospect.
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 for casting. In the figure: 1-casting the mould; 2-oil bath; 3-separating the net; 4-an ultrasonic generator; 5-the cavity. The ultrasonic generator is positioned at the bottom of the cavity, the die for casting is placed on the separation net in the cavity, and an oil bath is arranged in the cavity.
FIG. 2 shows that nano ZrB with 2 vol% is obtained by different preparation processes2Gold phase diagram of particulate aluminum matrix composite: (a) applying a conventional external field and adding no Gd element; (b) the external field application mode of the patent and the addition of 0.3 wt% of Gd element.
FIG. 3 shows that nano ZrB with 2 vol% is obtained by different preparation processes2Particle pattern of particulate aluminum matrix composite: (a) applying a conventional external field and adding no Gd element; (b) the external field application mode of the patent and the addition of 0.3 wt% of Gd element.
Detailed Description
The invention may be practiced according to, but is not limited to, the following examples; the terms used in the present invention, unless otherwise specified, generally have the meanings commonly understood by those of ordinary skill in the art; it will be understood that these examples are intended to illustrate the invention, and are not intended to limit the scope of the invention in any way; in the following examples, various procedures and methods not described in detail are conventional methods well known in the art.
The invention is further described below
Comparative example
Adopts a direct melt reaction method. 1247g of 6111 aluminum alloy is weighed, and K is weighed2ZrF6And KBF4And (3) respectively performing ball milling and refining on the powder, wherein the mass ratio of ball materials is 6: 1, the rotating speed is 300r/min, then the mixture is put into a vacuum drying oven, dried for 4 hours at 270 ℃, taken out, and the required K is calculated and weighed2ZrF6And KBF4(the mass ratio is 1: 1.08) as reactants, then fully mixing, and wrapping into a plurality of small bags by using aluminum foil paper for standby. Heating and melting 6111 aluminum alloy in a medium frequency induction furnace, heating to 870 deg.C, pressing the prepared reaction mixture into the melt with a graphite bell jar for reaction, then applying a magnetic field for electromagnetic regulation (the magnetic field frequency is 10Hz, the magnetic field strength is 0.08T, until the reaction is finished), reacting for 30min under the action of the magnetic field, skimming, and using C to remove slag2Cl6Refining and degassing to obtain a pure composite material melt, standing, pouring into a steel die preheated to 250 ℃ in a cavity of the device shown in the attached drawing 1 when the temperature reaches 760 ℃, wherein the ultrasonic frequency applied during the casting is 20000-25000Hz until the metal aluminum is cooled to about 500 ℃, namely the solidification is finished, and obtaining the composite material. Carrying out hot extrusion deformation processing on the prepared material, wherein the hot extrusion process comprises the following steps: the extrusion temperature is 480 ℃, the extrusion ratio is 16: 1, the extrusion speed is 4m/min, and the extruded sample is water-cooled. Then carrying out T6 heat treatment on the alloy, wherein the process parameters are as follows: the solid solution temperature is 520 ℃, the solid solution time is 6h, the pre-aging is carried out for 25min at 90 ℃ after the solid solution treatment, then the aging is carried out at 180 ℃, the aging time is 3h, and the water cooling is carried out to the normal temperature after the aging is finished. Then testing itTensile properties and fatigue properties.
Example 1
Preparation of 2 vol% ZrB2Nano-particle reinforced 0.08 wt.% rare earth modified aluminum-based composite material
Adopts a direct melt reaction method. Weighing 1253g of 6111 aluminum alloy, and weighing K2ZrF6And KBF4And (3) respectively performing ball milling and refining on the powder, wherein the mass ratio of ball materials is 6: 1, the rotating speed is 300r/min, then the mixture is put into a vacuum drying oven, dried for 4 hours at 270 ℃, taken out, and the required K is calculated and weighed2ZrF6And KBF4(the mass ratio is 1: 1.08) as reactants, then fully mixing, and wrapping into a plurality of small bags by using aluminum foil paper for standby. And (3) putting 6111 aluminum alloy into a medium-frequency induction furnace, heating and melting, heating to 750 ℃, adding 1.15g of Al-Gd alloy, preserving heat and standing for 5min to microalloy the Al-Gd alloy. Heating to 870 deg.C, pressing the prepared reaction mixture into melt with graphite bell jar for reaction, applying magnetic field for electromagnetic regulation (magnetic field frequency is 10Hz, magnetic field strength is 0.08T, magnetic field application manner is that the magnetic field is stopped for 1min after every 5min, then applying reverse magnetic field for 5min, circulating in sequence until the reaction is finished), reacting for 30min under the action of magnetic field, skimming slag, and reacting with C2Cl6Refining and degassing to obtain a pure composite material melt, standing, pouring into a steel die preheated to 250 ℃ in a cavity of the device shown in the attached drawing 1 when the temperature reaches 760 ℃, wherein the ultrasonic frequency applied during the casting is 20000-25000Hz until the metal aluminum is cooled to about 500 ℃, namely the solidification is finished, and obtaining the composite material. Carrying out hot extrusion deformation processing on the prepared material, wherein the hot extrusion process comprises the following steps: the extrusion temperature is 480 ℃, the extrusion ratio is 16: 1, the extrusion speed is 4m/min, and the extruded sample is water-cooled. Then carrying out T6 heat treatment on the alloy, wherein the process parameters are as follows: the solid solution temperature is 520 ℃, the solid solution time is 6h, the pre-aging is carried out for 25min at 90 ℃ after the solid solution treatment, then the aging is carried out at 180 ℃, the aging time is 3h, and the water cooling is carried out to the normal temperature after the aging is finished. The tensile and fatigue properties were then tested.
Example 2
Preparation of 2 vol% ZrB2Nanoparticle reinforced 0.15 wt.% rare earth modified aluminumBase composite material
Adopts a direct melt reaction method. 1206g of 6111 aluminum alloy is weighed, and K is weighed2ZrF6And KBF4And (3) respectively performing ball milling and refining on the powder, wherein the mass ratio of ball materials is 6: 1, the rotating speed is 300r/min, then the mixture is put into a vacuum drying oven, dried for 4 hours at 270 ℃, taken out, and the required K is calculated and weighed2ZrF6And KBF4(the mass ratio is 1: 1.08) as reactants, then fully mixing, and wrapping into a plurality of small bags by using aluminum foil paper for standby. The 6111 aluminum alloy is put into a medium frequency induction furnace to be heated and melted, the temperature is raised to 750 ℃, 2.08g of Al-Gd alloy is added, the temperature is kept and the mixture is kept still for 5min, and the microalloying is carried out. Heating to 870 deg.C, pressing the prepared reaction mixture into melt with graphite bell jar for reaction, applying magnetic field for electromagnetic regulation (magnetic field frequency is 10Hz, magnetic field strength is 0.08T, magnetic field application manner is that the magnetic field is stopped for 1min after every 5min, then applying reverse magnetic field for 5min, circulating in sequence until the reaction is finished), reacting for 30min under the action of magnetic field, skimming slag, and reacting with C2Cl6Refining and degassing to obtain a pure composite material melt, standing, pouring into a steel die preheated to 250 ℃ in a cavity of the device shown in the attached drawing 1 when the temperature reaches 760 ℃, wherein the ultrasonic frequency applied during the casting is 20000-25000Hz until the metal aluminum is cooled to about 500 ℃, namely the solidification is finished, and obtaining the composite material. Carrying out hot extrusion deformation processing on the prepared material, wherein the hot extrusion process comprises the following steps: the extrusion temperature is 480 ℃, the extrusion ratio is 16: 1, the extrusion speed is 4m/min, and the extruded sample is water-cooled. Then carrying out T6 heat treatment on the alloy, wherein the process parameters are as follows: the solid solution temperature is 520 ℃, the solid solution time is 6h, the pre-aging is carried out for 25min at 90 ℃ after the solid solution treatment, then the aging is carried out at 180 ℃, the aging time is 3h, and the water cooling is carried out to the normal temperature after the aging is finished. The tensile and fatigue properties were then tested.
Example 3
Preparation of 2 vol% ZrB2Nano-particle reinforced 0.3 wt.% rare earth modified aluminum-based composite material
Adopts a direct melt reaction method. 1230g of 6111 aluminum alloy is weighed, and K is weighed2ZrF6And KBF4Respectively ball-milling and refining the powderThe mass ratio of the ball material is 6: 1, the rotating speed is 300r/min, then the mixture is put into a vacuum drying oven, dried for 4 hours at 270 ℃, taken out, and the required K is calculated and weighed2ZrF6And KBF4(the mass ratio is 1: 1.08) as reactants, then fully mixing, and wrapping into a plurality of small bags by using aluminum foil paper for standby. And (3) putting 6111 aluminum alloy into a medium-frequency induction furnace, heating and melting, heating to 750 ℃, adding 4.24g of Al-Gd alloy, preserving heat and standing for 5min to microalloy the Al-Gd alloy. Heating to 870 deg.C, pressing the prepared reaction mixture into melt with graphite bell jar for reaction, applying magnetic field for electromagnetic regulation (magnetic field frequency is 10Hz, magnetic field strength is 0.08T, magnetic field application manner is that the magnetic field is stopped for 1min after every 5min, then applying reverse magnetic field for 5min, circulating in sequence until the reaction is finished), reacting for 30min under the action of magnetic field, skimming slag, and reacting with C2Cl6Refining and degassing to obtain a pure composite material melt, standing, pouring into a steel die preheated to 250 ℃ in a cavity of the device shown in the attached drawing 1 when the temperature reaches 760 ℃, wherein the ultrasonic frequency applied during the casting is 20000-25000Hz until the metal aluminum is cooled to about 500 ℃, namely the solidification is finished, and obtaining the composite material. Carrying out hot extrusion deformation processing on the prepared material, wherein the hot extrusion process comprises the following steps: the extrusion temperature is 480 ℃, the extrusion ratio is 16: 1, the extrusion speed is 4m/min, and the extruded sample is water-cooled. Then carrying out T6 heat treatment on the alloy, wherein the process parameters are as follows: the solid solution temperature is 520 ℃, the solid solution time is 6h, the pre-aging is carried out for 25min at 90 ℃ after the solid solution treatment, then the aging is carried out at 180 ℃, the aging time is 3h, and the water cooling is carried out to the normal temperature after the aging is finished. The tensile and fatigue properties were then tested.
Example 4
Preparation of 2 vol% ZrB2Nano-particle reinforced 0.45 wt.% rare earth modified aluminum-based composite material
Adopts a direct melt reaction method. Weighing 1216g of 6111 aluminum alloy, and weighing K2ZrF6And KBF4And (3) respectively performing ball milling and refining on the powder, wherein the mass ratio of ball materials is 6: 1, the rotating speed is 300r/min, then the mixture is put into a vacuum drying oven, dried for 4 hours at 270 ℃, taken out, and the required K is calculated and weighed2ZrF6And KBF4(Mass)The quantity ratio is 1: 1.08) as reactants, then fully mixing, and wrapping into a plurality of small bags by using aluminum foil paper for standby. And (3) putting 6111 aluminum alloy into a medium-frequency induction furnace, heating and melting, heating to 750 ℃, adding 6.29g of Al-Gd alloy, preserving heat and standing for 5min to microalloy the Al-Gd alloy. Heating to 870 deg.C, pressing the prepared reaction mixture into melt with graphite bell jar for reaction, applying magnetic field for electromagnetic regulation (magnetic field frequency is 10Hz, magnetic field strength is 0.08T, magnetic field application manner is that the magnetic field is stopped for 1min after every 5min, then applying reverse magnetic field for 5min, circulating in sequence until the reaction is finished), reacting for 30min under the action of magnetic field, skimming slag, and reacting with C2Cl6Refining and degassing to obtain a pure composite material melt, standing, pouring into a steel die preheated to 250 ℃ in a cavity of the device shown in the attached drawing 1 when the temperature reaches 760 ℃, wherein the ultrasonic frequency applied during the casting is 20000-25000Hz until the metal aluminum is cooled to about 500 ℃, namely the solidification is finished, and obtaining the composite material. Carrying out hot extrusion deformation processing on the prepared material, wherein the hot extrusion process comprises the following steps: the extrusion temperature is 480 ℃, the extrusion ratio is 16: 1, the extrusion speed is 4m/min, and the extruded sample is water-cooled. Then carrying out T6 heat treatment on the alloy, wherein the process parameters are as follows: the solid solution temperature is 520 ℃, the solid solution time is 6h, the pre-aging is carried out for 25min at 90 ℃ after the solid solution treatment, then the aging is carried out at 180 ℃, the aging time is 3h, and the water cooling is carried out to the normal temperature after the aging is finished. The tensile and fatigue properties were then tested.
The composite material examples obtained in the examples and the composite material without rare earth are extruded and deformed, then processed into tensile samples according to the method of a GB28-2002 metal material room temperature tensile test, subjected to solution treatment at 525 ℃ for 2h, subjected to water quenching, and subjected to heat preservation at 175 ℃ for 4h, and the tensile mechanical property at room temperature is tested by using an AGS-X universal testing machine after the temperature is reduced to the room temperature.
TABLE 1 mechanical Properties of the composites after Heat treatment
| Test number | Tensile strength (MPa) | Elongation (%) | Yield strength | Fatigue strength |
| Comparative example | 343 | 20.3 | 264 | 85MPa |
| Example 1 | 362 | 21.6 | 285 | 90MPa |
| Example 2 | 369 | 23.5 | 296 | 100MPa |
| Example 3 | 378 | 27.8 | 309 | 115MPa |
| Example 4 | 360 | 26.5 | 282 | 105MPa |
As can be seen from Table 1, the tensile strength of the composite material of the comparative example is 343MPa, the elongation is 20.3%, the yield strength is 264MPa, the tensile strength of the composite material of example 3 is 378MPa, the elongation is 27.8%, the yield strength is 309MPa, the tensile strength is improved by 10.2%, the plasticity is improved by 36.9%, the yield strength is improved by 17.0%, and the fatigue strength is improved by 35.3% compared with the comparative example. Therefore, the process can stably prepare the high-toughness anti-fatigue in-situ aluminum-based composite material, and has great application potential in the fields of aviation, automobiles and the like
After the comparative example and the example 3 are ground and polished, the microstructure of the composite material is observed by a metallographic microscope, as shown in the attached figure 2, the composite material prepared in the example 3 has the advantages that compared with the structure of the comparative example, the crystal grains are obviously refined, and the particle distribution is more uniform.
After the comparative example and the example 3 are polished, the morphology and the distribution of the nano particles are observed by using SEM, as shown in figure 3, it can be seen that the particles of the composite material prepared by the example 3 are round and are uniformly distributed.
Claims (3)
1. A preparation method of a high-strength, high-toughness and anti-fatigue in-situ aluminum-based composite material is characterized in that an Al-Zr-B system is adopted to prepare a particle-reinforced aluminum-based composite material, and the added reactant is K2ZrF6And KBF4Powder preparation; 6111 aluminum alloy is taken as a matrix;
firstly, respectively carrying out vacuum ball milling on two kinds of villiaumites, then placing the villiaumites into a vacuum drying oven to remove crystal water, weighing the required villiaumites according to the volume fraction of generated particles after drying, uniformly mixing the villiaumites, then wrapping the villiaumites into small bags by using aluminum foil paper for standby, and adding the reaction villiaumites according to ZrB2The volume fraction of the particles in the finally obtained high-toughness anti-fatigue in-situ aluminum-based composite material is 1-3 percent;
melting 6111 aluminum alloy, heating to 730-750 ℃, adding Mg-Gd alloy,microalloying the alloy, wherein the mass fraction of Gd in the Mg-Gd alloy is 87 percent, and the addition amount of Gd is 0.05-0.5 percent of the mass of AA 6111; continuously heating to 850-870 ℃, pressing the prepared villiaumite into the aluminum alloy solution by using a graphite bell jar, then applying a magnetic field for electromagnetic regulation and control, and reacting for 20-30min under the action of the magnetic field; after the reaction is finished, slagging off, refining and degassing are carried out, pouring is carried out in an ultrasonic forming device when the temperature is reduced to 730-2A particle-reinforced aluminum-based composite material;
rare earth modified ZrB2Carrying out hot extrusion deformation processing on the particle reinforced aluminum matrix composite, and testing the tensile property and the fatigue property through a T6 heat treatment process; the hot extrusion process comprises the following steps: the extrusion temperature is 440-500 ℃, the extrusion ratio is 16: 1, extruding at the speed of 3-5m/min, and carrying out water cooling on an extruded sample; the T6 heat treatment process parameters are as follows: the solid solution temperature is 500-530 ℃, the solid solution time is 3-12h, the pre-aging is carried out at 80-100 ℃ after the solid solution treatment, the aging is carried out at 170-185 ℃, the aging time is 1-5h, and the water cooling is carried out to the normal temperature after the aging is finished;
the magnetic field applied by the electromagnetic regulation and control is a multi-section alternating magnetic field, so that the problem of centrifugal agglomeration of particles caused by a continuous directional magnetic field is solved, and the particles are more uniformly distributed; the frequency of the magnetic field is 8-17Hz, the intensity of the magnetic field is 0.03-0.09T, and the application mode of the magnetic field is as follows: stopping for 0.5-1min after applying the magnetic field for 4-6min, then applying the reverse magnetic field for 4-6min, and circulating in sequence until the reaction is finished;
the ultrasonic forming device comprises a die for casting, an oil bath, an ultrasonic generator and a cavity; the ultrasonic generator is positioned at the bottom of the cavity, the die used for casting is placed on the separation net in the cavity, and an oil bath is arranged in the cavity; the specific steps of applying the ultrasound during casting are that before casting, the mould is placed in the device cavity, the mould is in an ultrasound field, the mould is preheated to 250 ℃ under the action of an oil bath in the device cavity, and the ultrasound frequency applied during casting is 20000-.
2. The preparation method of the high-toughness anti-fatigue in-situ aluminum-based composite material as claimed in claim 1, wherein the 6111 alloy comprises the following chemical components by mass percent: si: 0.6-1.1%, Mg: 0.5-1.1%, Cu: 0.5-0.9%, Fe <0.4%, Mn 0.1-0.45%, Zn: <0.15, the balance being Al.
3. The preparation method of the high-strength-toughness anti-fatigue in-situ aluminum-based composite material as claimed in claim 1, wherein the KBF is prepared by using a conventional method4And K2ZrF6The mass ratio of (A) to (B) is 1: 1.08; the ZrB2The size of the particles is 50-90nm, and the morphology of the particles is quadrilateral or hexagonal.
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