CN110257655B - High-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material and preparation method thereof - Google Patents

High-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material and preparation method thereof Download PDF

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CN110257655B
CN110257655B CN201910604000.5A CN201910604000A CN110257655B CN 110257655 B CN110257655 B CN 110257655B CN 201910604000 A CN201910604000 A CN 201910604000A CN 110257655 B CN110257655 B CN 110257655B
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tib
alloy
ultrasonic
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melt
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CN110257655A (en
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刘志伟
赵樱
郑巧玲
皇志富
高义民
邢建东
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Xian Jiaotong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/20Measures not previously mentioned for influencing the grain structure or texture; Selection of compositions therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making alloys by melting
    • C22C1/026Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making alloys by melting
    • C22C1/03Making alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/003Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-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
    • C22C32/0047Non-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
    • C22C32/0073Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides

Abstract

The invention discloses a high-dispersion distribution nano TiB2A particle reinforced Al-base composite material is prepared through ultrasonic aided reaction of mixed salt (K)2TiF6/KBF4Al) to prepare Al-TiB with uniform structure2Master alloy in which TiB is grown in situ2Average particle diameter of the particles<100 nm. With Al-TiB2The intermediate alloy and Al are used as raw materials, or Al-TiB is used as2Taking intermediate alloy, Al and alloy elements as raw materials, and diluting the nano TiB by an intermediate alloy dilution method2Introducing particles into an aluminum (alloy) matrix, performing ultrasonic stirring treatment, pouring into a mold, and applying ultrasonic waves (introduced by a bottom introduction method) in the solidification process to obtain high-dispersion-distribution nano TiB2A particulate reinforced aluminum matrix composite.

Description

High-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material and preparation method thereof
Technical Field
The invention belongs to the field of advanced metal matrix composite material preparation, and particularly relates to a method for preparing high-dispersion distribution nano TiB by an ultrasonic-assisted liquid phase composite method2A method for reinforcing aluminum-based composite material by using granular ceramic particles.
Background
The nano ceramic particles are introduced into the aluminum melt by a liquid phase composite method and are solidified to prepare the nano ceramic particle/aluminum matrix composite material. The nano ceramic particles have refining and strengthening effects on an aluminum alloy solidification structure, can greatly improve the specific strength, specific modulus and thermal fatigue resistance of the alloy, and have very wide application prospects in the fields of aerospace, automobile manufacturing, electronic devices, sports equipment and the like. In addition, the liquid phase composite method has the advantages of low production cost, suitability for large-scale production and the like, so the process has great attention in the field of preparation of the nano ceramic particle/aluminum-based composite material. However, the ceramic phase has poor wettability with aluminum melt, which is extremely disadvantageous for the preparation of high-quality nano ceramic particle/aluminum matrix composite materials. On one hand, the traditional particle adding method (assisted by mechanical stirring) is difficult to completely introduce the nano ceramic particles into the aluminum melt; on the other hand, in conventional solidification (gravity casting), the nano ceramic particles are mostly deviated and polymerized at alpha-Al crystal boundaries (crystal boundaries for short) under the repulsion action of a solid-liquid interface, so that the particles are deviated and polymerized on the crystal boundaries on a large scale, the hot cracking tendency of the material is easily increased, the plasticity and toughness of the material are seriously reduced, the potential safety hazard of the use of the material is caused, and the popularization and the application of the material are limited.
Disclosure of Invention
The invention aims to provide a high-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material and a preparation method thereof, which are used for overcoming the defects in the prior art and can obtain high-dispersion-distribution nano TiB2A particulate reinforced aluminum matrix composite.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material comprises the following steps:
step 1: will K2TiF6、KBF4Mixing the powder according to the molar ratio of 1:2, adding the mixture into a pure aluminum melt, and performing ultrasonic stirring treatment to prepare Al-TiB with uniform tissue2Master alloy, and Al-TiB obtained2Intermediate alloy of TiB2The average particle size of the particles is less than 100 nm;
step 2: al and Al-TiB prepared in step 12Taking an intermediate alloy as a raw material, or taking Al, alloy elements and Al-TiB prepared in the step 12The intermediate alloy is used as a raw material, the raw material is melted, ultrasonic stirring is used for processing dispersed particles in the melting process, and TiB-containing particles are obtained2A particulate aluminum melt;
and step 3: the TiB-containing material obtained in the step 22Pouring the granular aluminum melt into a mold, introducing ultrasonic waves by a bottom introduction method in the melt solidification process, and obtaining high-dispersion-distribution nano TiB after solidification2A particulate reinforced aluminum matrix composite.
Further, the temperature of the pure aluminum melt in the step 1 is 700-.
Further, the ultrasonic agitation treatment in the step 1 specifically comprises: and immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, wherein the ultrasonic treatment time is 5-10min, and the ultrasonic power is 0.5-1.5 kW.
Further, the obtained Al-TiB2Intermediate alloy of TiB2The mass fraction of the particles is less than or equal to 15 percent.
Further, in step 2, the raw materials are melted at 800 ℃ at 700-.
Further, the ultrasonic agitation treatment in the step 2 specifically comprises: and immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, wherein the ultrasonic treatment time is 5-10min, and the ultrasonic power is 0.5-1.5 kW.
Further, the introduction of ultrasound by the bottom introduction method in step 3 is specifically: and (3) penetrating an ultrasonic amplitude rod made of Nb-Zr alloy through the bottom of the die, and contacting the ultrasonic amplitude rod with the melt in the solidification process, wherein the ultrasonic power is 0.5-1.5kW, and the ultrasonic time is the solidification time.
A high-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material is prepared by adopting the preparation method of the high-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention utilizes ultrasonic-assisted mixed salt reaction, can remarkably accelerate the mixed salt reaction process by cavitation and acoustic flow effects generated in the aluminum melt by high-strength ultrasonic, and can synthesize TiB with the average grain diameter of less than 100nm at lower temperature (lower than 850 ℃) in shorter time (less than 10min)2Particles of and TiB2The yield of the particles can reach more than 90% (no other impurity phase exists). When the traditional mixed salt reaction process (without ultrasonic assistance) is adopted, the melt temperature needs to be higher than 850 ℃, the reaction time needs to be more than 30min (in order to ensure the synthesis rate of TiB2 particles), and the size of the obtained TiB2 particles is submicron and micron particle size. Therefore, the particle size of TiB2 can be obviously reduced by adopting ultrasonic assistance, and the production cost can be effectively reduced. In addition, the stirring effect generated by the ultrasonic in the aluminum melt can effectively break the TiB2The particle agglomeration and the ultrasonic cavitation effect can obviously improve the TiB2The particles and the aluminum melt are fully dispersed in the melt due to the wettability, the ultrasonic treatment has the functions of degassing and impurity removal, and the aluminum melt can be pouredThe Al-TiB with uniform structure and less pores/inclusions is obtained2And (3) intermediate alloy. The result can realize the controllable preparation of the subsequent composite material (TiB in the composite material)2The content of the particles is controllable), thereby obtaining high-dispersion distribution nano TiB2A particulate reinforced aluminum matrix composite.
The ultrasonic amplitude rod used in the invention is made of Nb-Zr alloy material, and has more stability (the solubility of niobium in the aluminum melt is extremely low) in the aluminum melt compared with the traditional Ti alloy, and can effectively avoid introducing other alloy elements into the aluminum melt.
The ultrasonic wave is introduced into the solidification of the composite material through a bottom introduction method, on one hand, the TiB can be obviously improved through the ultrasonic wave in the alpha-Al nucleation stage2The wettability of the particles and the melt and the ultrasonic field can make the melt temperature/solute field more uniform, and the nucleation capability of the particles as heterogeneous nucleation (more TiB)2The particles may be nucleated intragranular by α -Al); on the other hand, in the growth stage of alpha-Al, the ultrasonic field can accelerate the propelling speed of a solid-liquid interface, which is beneficial to TiB2The particles are trapped by the solid-liquid interface (more TiB2The particles enter the crystal). In addition, the acoustic flow effect generated by the ultrasonic field can avoid the nano TiB in solidification2The particles precipitate in the melt. The ultrasonic field can also effectively refine the solidification structure of the aluminum matrix, and the refinement of the matrix grains can further improve the dispersibility of the TiB2 nanoparticles. In conclusion, the invention can obviously improve the nano TiB2Dispersibility of the particles in the aluminum matrix.
Drawings
FIG. 1 shows Al-TiB prepared in example 12Microstructure picture and phase XRD diffraction pattern of intermediate alloy, wherein (a) is microstructure appearance of intermediate alloy, (b) is phase XRD analysis of intermediate alloy, (c) is grain appearance and phase XRD analysis of extracted TiB2, and (d) is TiB2And (4) analyzing the particle size.
FIG. 2 shows the preparation of nano-TiB by conventional coagulation (without ultrasound) and ultrasound-assisted coagulation in example 12The microstructure picture of the particle reinforced aluminum-based composite material is shown in the specification, wherein (a) the microstructure appearance of the conventional solidification (no ultrasonic) composite material is shown in the specification, and (b) the microstructure appearance of the ultrasonic auxiliary solidification composite material is shown in the specification。
Detailed Description
Embodiments of the invention are described in further detail below:
high-dispersion-distribution nano TiB2The invention relates to a method for preparing particle reinforced aluminum-based composite material, which firstly utilizes ultrasonic-assisted mixed salt reaction (K)2TiF6/KBF4Al) to prepare Al-TiB with uniform structure2Master alloy in which TiB is grown in situ2Average particle diameter of the particles<100 nm. With Al-TiB2The intermediate alloy, Al and alloy elements are used as raw materials, or Al-TiB is used as2Taking intermediate alloy and Al as raw materials, and diluting the nano TiB by the intermediate alloy dilution method2The particles are introduced into an aluminum (alloy) matrix and assisted by ultrasonic stirring, then the aluminum (alloy) matrix is poured into a mold, and ultrasonic waves are applied during solidification (introduced by a bottom introduction method), so that high-dispersion distribution nano TiB is obtained2A particulate reinforced aluminum matrix composite.
The method specifically comprises the following steps:
step 1: will K2TiF6、KBF4Mixing the powder according to the molar ratio of 1:2, adding the mixed powder into a pure aluminum melt with the temperature of 700-plus-one 850 ℃, performing ultrasonic stirring treatment to remove liquid molten salt impurities on the surface of the melt, and preparing Al-TiB with uniform tissue after pouring2Master alloy of which TiB2The average particle diameter of the particles is less than 100nm, and the obtained Al-TiB2Intermediate alloy of TiB2The mass fraction of the particles is less than or equal to 15 percent.
Step 2: al and Al-TiB prepared in step 12Taking an intermediate alloy as a raw material, or taking Al, alloy elements and Al-TiB prepared in the step 12The intermediate alloy is used as raw material, in which the alloy elements are Si, Mg, Cu, Zn, etc. (alloy elements commonly used for casting and deforming aluminium alloy), and different TiB are prepared by regulating and controlling the proportion2The aluminum-based composite material with particle content is prepared by melting the raw materials at the temperature of 700-800 ℃, and dispersing particles by ultrasonic stirring to obtain the TiB-containing material2A particulate aluminum melt.
And step 3: the step 2 contains TiB2Pouring the granular aluminum melt into a mold, and introducing the molten aluminum melt into the mold during solidification of the molten aluminum meltIntroducing ultrasonic wave through bottom introduction method, and solidifying to obtain high-dispersion-distribution nano TiB2A particulate reinforced aluminum matrix composite.
The adding mode of ultrasonic auxiliary stirring adopted in the steps 1 and 2 is as follows: immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, wherein the ultrasonic treatment time is 5-10min, the ultrasonic power is 0.5-1.5kW, and the K is controlled in the step 12TiF6、KBF4The addition amount of the powder can be used for preparing different TiB2Particle content of Al-TiB2Intermediate alloy, introduction mode of ultrasound in step 3: and (3) enabling an Nb-Zr ultrasonic amplitude rod to pass through the bottom of the die and contact with the melt during solidification, wherein the ultrasonic power is 0.5-1.5kW, and the ultrasonic time is the solidification time.
The present invention is described in further detail below with reference to examples:
example 1
Step 1: will K2TiF6、KBF4Mixing the powder according to a molar ratio of 1:2, fully mixing, adding the mixture into a pure aluminum melt at the temperature of 800 ℃, simultaneously immersing an Nb-Zr alloy ultrasonic amplitude rod into the melt, carrying out ultrasonic treatment for 10min with the ultrasonic power of 1.2kW, removing liquid molten salt impurities on the surface of the melt, and pouring to obtain Al-TiB2Master alloy, Al-TiB obtained2Intermediate alloy of TiB2The mass fraction of the particles was 10%.
Step 2: with Al-TiB2Taking intermediate alloy and Al as raw materials to prepare 3 wt.% of TiB2Particle reinforced aluminum matrix composite (TiB)2TiB in particle reinforced aluminum-based composite material2The mass fraction of the particles is 3%), melting at 750 deg.C, and ultrasonic processing for 5min with ultrasonic power of 1.2 kW.
And step 3: pouring the molten aluminum-based composite material into a steel mold, introducing ultrasound through a bottom introduction method, wherein the ultrasound power is 1.2kW, and solidifying to obtain the nano TiB2A particulate reinforced aluminum matrix composite.
FIG. 1 shows Al-10TiB prepared by ultrasound-assisted mixed salt reaction2The microstructure of the master alloy is uniform (a) and no other reinforcing phase is generated (b). In situ endogenous TiB2Average of particles(c) - (d) having a particle size of less than 100 nm.
FIG. 2 (a) shows that nano TiB is solidified in the conventional way2The particles are mainly segregated in the alpha-Al crystal boundary, and (b) shows that the ultrasonic-assisted solidification can effectively improve the TiB2Dispersibility of the particles.
Example 2
Step 1: will K2TiF6、KBF4Mixing the powder according to a molar ratio of 1:2, fully mixing, adding the mixture into a pure aluminum melt at the temperature of 750 ℃, simultaneously immersing an Nb-Zr alloy ultrasonic amplitude rod into the melt, carrying out ultrasonic treatment for 10min with the ultrasonic power of 1.0kW, removing liquid molten salt impurities on the surface of the melt, and pouring to obtain Al-TiB2Master alloy, Al-TiB obtained2Intermediate alloy of TiB2The mass fraction of the particles was 5%.
Step 2: with Al-TiB2Taking intermediate alloy and Al as raw materials to prepare 5 wt.% of TiB2Particle reinforced aluminum matrix composite (TiB)2TiB in particle reinforced aluminum-based composite material2The mass fraction of the particles is 5%), melting at 800 deg.C, and ultrasonic processing for 5 min.
And step 3: pouring the molten aluminum-based composite material into a steel mold, introducing ultrasound through a bottom introduction method, wherein the ultrasound power is 1.0kW, and solidifying to obtain the nano TiB2A particulate reinforced aluminum matrix composite.
Example 3
Step 1: will K2TiF6、KBF4Mixing the powder according to the molar ratio of 1:2, fully mixing, adding the mixture into a pure aluminum melt at the temperature of 700 ℃, simultaneously immersing an Nb-Zr alloy ultrasonic amplitude rod into the melt, carrying out ultrasonic treatment for 10min with the ultrasonic power of 1.5kW, removing liquid molten salt impurities on the surface of the melt, and pouring to obtain Al-TiB2Master alloy, Al-TiB obtained2Intermediate alloy of TiB2The mass fraction of the particles was 15%.
Step 2: with Al-TiB2Intermediate alloy and Al are used as raw materials to prepare 7 wt.% of TiB2Particle reinforced aluminum matrix composite (TiB)2TiB in particle reinforced aluminum-based composite material2The mass fraction of the particles is 7%),melting at 750 deg.C, and treating with ultrasound for 5min with ultrasonic power of 1.5 kW.
And step 3: pouring the molten aluminum-based composite material into a steel mold, introducing ultrasound through a bottom introduction method, wherein the ultrasound power is 0.5kW, and solidifying to obtain the nano TiB2A particulate reinforced aluminum matrix composite.
Example 4
Step 1: will K2TiF6、KBF4Mixing the powder according to a molar ratio of 1:2, fully mixing, adding the mixture into a pure aluminum melt with the temperature of 850 ℃, simultaneously immersing an Nb-Zr alloy ultrasonic amplitude rod into the melt, carrying out ultrasonic treatment for 8min with the ultrasonic power of 1.0kW, removing liquid molten salt impurities on the surface of the melt, and pouring to obtain Al-TiB2Master alloy, Al-TiB obtained2Intermediate alloy of TiB2The mass fraction of the particles was 1%.
Step 2: with Al-TiB2Intermediate alloy and Al are used as raw materials to prepare 10 wt.% of TiB2Particle reinforced aluminum matrix composite (TiB)2TiB in particle reinforced aluminum-based composite material2The mass fraction of the particles is 10%), melting at 700 deg.C, and treating with ultrasound for 10min, with an ultrasonic power of 1.0 kW.
And step 3: pouring the molten aluminum-based composite material into a steel mold, introducing ultrasound through a bottom introduction method, wherein the ultrasound power is 1.0kW, and solidifying to obtain the nano TiB2A particulate reinforced aluminum matrix composite.
Example 5
Step 1: will K2TiF6、KBF4Mixing the powder according to a molar ratio of 1:2, fully mixing, adding the mixture into a pure aluminum melt with the temperature of 850 ℃, simultaneously immersing an Nb-Zr alloy ultrasonic amplitude rod into the melt, carrying out ultrasonic treatment for 5min with the ultrasonic power of 0.5kW, removing liquid molten salt impurities on the surface of the melt, and pouring to obtain Al-TiB2Master alloy, Al-TiB obtained2Intermediate alloy of TiB2The mass fraction of the particles was 10%.
Step 2: with Al-TiB2Taking intermediate alloy, Al and alloy element Si as raw materials to prepare 3 wt.% of TiB2Particle size increasingStrong aluminium base composite material (TiB)2TiB in particle reinforced aluminum-based composite material2The mass fraction of the particles is 3%), melting at 700 deg.C, and treating with ultrasound for 8min, with an ultrasonic power of 0.5 kW.
And step 3: pouring the molten aluminum-based composite material into a steel mold, introducing ultrasound through a bottom introduction method, wherein the ultrasound power is 1.5kW, and solidifying to obtain the nano TiB2A particulate reinforced aluminum matrix composite.
Wherein, the alloy element Si can also adopt Mg, Cu, Zn and the like (common alloy elements for casting and deforming aluminum alloy).

Claims (5)

1. A preparation method of a high-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material is characterized by comprising the following steps:
step 1: will K2TiF6、KBF4Mixing the powder according to the molar ratio of 1:2, adding the mixture into a pure aluminum melt, and performing ultrasonic stirring treatment to prepare Al-TiB with uniform tissue2Master alloy, and Al-TiB obtained2Intermediate alloy of TiB2The average particle size of the particles is less than 100 nm;
wherein the ultrasonic stirring treatment specifically comprises the following steps: immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, wherein the ultrasonic treatment time is 5-10min, and the ultrasonic power is 0.5-1.5 kW;
step 2: al and Al-TiB prepared in step 12Taking an intermediate alloy as a raw material, or taking Al, alloy elements and Al-TiB prepared in the step 12The intermediate alloy is used as a raw material, the raw material is melted, ultrasonic stirring is used for processing dispersed particles in the melting process, and TiB-containing particles are obtained2A particulate aluminum melt;
wherein the ultrasonic stirring treatment specifically comprises the following steps: immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, wherein the ultrasonic treatment time is 5-10min, and the ultrasonic power is 0.5-1.5 kW;
and step 3: the TiB-containing material obtained in the step 22Pouring the granular aluminum melt into a mold, introducing ultrasonic waves by a bottom introduction method in the melt solidification process, and obtaining high-dispersion-distribution nano TiB after solidification2A particle-reinforced aluminum-based composite material;
the introduction of ultrasound by the bottom introduction method specifically comprises the following steps: and (3) penetrating an ultrasonic amplitude rod made of Nb-Zr alloy through the bottom of the die, and contacting the ultrasonic amplitude rod with the melt in the solidification process, wherein the ultrasonic power is 0.5-1.5kW, and the ultrasonic time is the solidification time.
2. The method for preparing the high-dispersion-distribution nano titanium diboride particle-reinforced aluminum-based composite material as claimed in claim 1, wherein the pure aluminum melt temperature in step 1 is 700-.
3. The method for preparing the high-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material as claimed in claim 1, wherein the obtained Al-TiB2Intermediate alloy of TiB2The mass fraction of the particles is less than or equal to 15 percent.
4. The method for preparing the high-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material as claimed in claim 1, wherein the raw materials are melted at the temperature of 700-800 ℃ in the step 2.
5. A high-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material is characterized by being prepared by the preparation method of the high-dispersion-distribution nano titanium diboride particle reinforced aluminum-based composite material as claimed in any one of claims 1 to 4.
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