CN106312057B - Powder metallurgy preparation method of nano-particle reinforced superfine crystal metal matrix composite material - Google Patents
Powder metallurgy preparation method of nano-particle reinforced superfine crystal metal matrix composite material Download PDFInfo
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Abstract
The invention provides a powder metallurgy preparation method of a nano-particle reinforced ultrafine-grained metal matrix composite, which comprises the following steps of: firstly, preparing micro-nano flaky metal matrix powder in advance; mixing the nano particles and the flaky metal matrix powder in a stirrer at a high speed in a protective atmosphere, and uniformly dispersing the nano particles on the surface of the micro-nano flaky metal matrix powder by using high shear force and pressure generated between a stirring blade and a tank body; embedding nano metal particles into micro-nano flaky metal matrix powder through short-time mechanical ball milling treatment to obtain composite powder of nano particle reinforced metal; the superfine crystal metal matrix composite with uniformly dispersed nano particles is obtained through compression molding, sintering and densification treatment. The invention saves time and energy, has low cost and wide application range, and the prepared material has high comprehensive mechanical property and large-scale application potential.
Description
Technical Field
The invention relates to the technical field of metal matrix composite materials, in particular to a powder metallurgy preparation method of a nanoparticle reinforced ultrafine grain metal matrix composite material.
Background
The metal matrix composite material compounded by the metal matrix and the reinforcement has the characteristics of metal ductility, high hardness, high modulus and the like of the reinforcement, and has important application and irreplaceability in high-tech fields such as transportation, aerospace and the like. With the further development of science and technology, the high-tech fields such as transportation, aerospace and the like also put forward higher requirements on the comprehensive performance of the metal-based composite material, and the nanocrystallization of the reinforcement particles and the ultrafine grain nanocrystalline reinforcement of the metal matrix are the development directions of a new generation of metal-based composite material, so that the development of the preparation technology of the nanoparticle reinforced ultrafine grain composite material is a hot point of domestic and foreign research.
According to the search of technical documents, the main technical means of the nano-particle reinforced ultrafine grained metal matrix composite material at present can be divided into two categories. The first is a liquid method, firstly dispersing nano particles into a melt, and then applying large plastic deformation to a bulk material obtained by solidification so as to refine crystal grains and make the distribution of the nano particles more uniform; the second type is a mechanical alloying method in powder metallurgy, namely, spherical metal powder and nano reinforcement particles are mechanically mixed and then subjected to long-time high-energy ball milling, the nano particles of clusters are gradually dispersed into a matrix through repeated cold welding and crushing processes of the powder, and meanwhile, crystal grains of matrix metal are refined into ultrafine crystals. Finally, preparing the bulk composite material through densification processes such as sintering, extrusion and the like. In the liquid method, the nano particles are easy to be deviated to a crystal boundary in the solidification process, and the existence of the nano particles greatly hinders the deformation of the matrix, so that the deformation is easy to be uneven, and the requirement on deformation processing equipment is high. The mechanical alloying method has the advantages of strong designability and wide application range, and becomes a main method for preparing the massive nano-particle reinforced superfine crystal composite material. Although the mechanical alloying method can better realize the dispersion of the nano particles, the mechanical alloying method also has the following defects: the original metal powder is usually spherical powder with the size of tens of microns, has large size difference with the nano reinforcement, and requires long-time ball millingThe process realizes grain refinement and dispersion, is time-consuming and labor-consuming, and is easy to cause local nano-particles to re-agglomerate; for example, the mixture of 50 μm diameter aluminum powder and 5 vol.% of 35nm diameter Al powder (Hesabi Z R, Materials Science and Engineering: A,2006,428(1):159-2O3The particles are directly mixed and ball-milled in a planetary ball mill at 250 r/min for 24 hours, and the nano particles are found to be agglomerated on the surface of the aluminum particles in the early stage (within 8 hours) of ball milling, and the ball milling time is more than 20 hours to ensure that the nano Al can be obtained2O3The particles are embedded in the aluminum matrix well and reach a stable state. Nevertheless, many nanoparticles are still agglomerated together, resulting in poor strengthening effect. The prior mechanical alloying technology has the following defects: in the initial stage of ball milling, the nanoparticles are wrapped in the matrix powder in the form of clusters, which requires a long time of ball milling, i.e., repeated large deformation process of the matrix metal powder, to further disperse the nanoparticles in the matrix. The total ball milling time is long and the energy consumption is high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a powder metallurgy preparation method of a nano-particle reinforced ultrafine-grained metal-based composite material, and the composite material prepared by the method has the characteristics of fine metal matrix grains and uniform dispersion of a nano reinforcement, has good matching of strength and plasticity and toughness, and has obviously improved comprehensive mechanical properties compared with the conventional powder metallurgy.
In order to achieve the purpose, the invention adopts the following technical scheme:
a powder metallurgy preparation method of a nanoparticle reinforced ultrafine grained metal matrix composite material is characterized in that a metal matrix grain refinement process and a nanoparticle dispersion process are carried out step by step, and the method comprises the following steps: firstly, preparing micro-nano flaky metal matrix powder in advance; then, stirring and mixing the nano particles and the micro-nano flaky metal matrix powder in a stirrer at a high speed for a short time under a protective atmosphere, and uniformly dispersing the nano particles on the surface of the micro-nano flaky metal matrix powder by utilizing high shearing force and pressure generated between a stirring blade and a tank body; further embedding the nano particles into micro-nano flaky metal matrix powder through short-time mechanical ball milling treatment to obtain nano particle reinforced metal composite particles; finally, the superfine crystal metal matrix composite with uniformly dispersed nano particles is obtained through compression molding, sintering and densification treatment.
Specifically, the method comprises the following steps:
the method comprises the following steps:
(1) ball-milling the spherical metal matrix powder to obtain micro-nano flaky metal matrix powder with a large specific surface area, and simultaneously reducing the grain size of the metal matrix to an ultra-fine grain range;
(2) adding the micro-nano flaky metal matrix powder obtained in the step (1) and nano particles into a stirrer according to a design proportion, and uniformly dispersing the nano particles on the surface of the micro-nano flaky metal matrix powder by high-speed stirring and mixing under a protective atmosphere to obtain mixed powder with uniformly dispersed nano particles;
(3) performing short-time mechanical ball milling treatment on the mixed powder obtained in the step (2) to enable nano particles to be embedded into micro-nano flaky metal matrix powder, so as to obtain composite powder with uniformly dispersed nano particles;
(4) and (4) performing pressing, blank forming, sintering and densification treatment on the composite powder obtained in the step (3) to obtain the nano-particle reinforced superfine crystal metal matrix composite material.
Preferably, in (1), the diameter of the spherical metal matrix powder is between 1 and 100 μm;
preferably, in the step (1), the grain size of the micro-nano flaky metal matrix powder obtained after ball milling is 50-500 nm, the specific surface area is 10-30 times of that of the original spherical metal matrix powder, the thickness is 0.1-2 μm, and the sheet diameter is 5-500 μm.
Preferably, the ball milling process is wet milling or dry milling, and the wet milling solvent is one selected from water, ethanol or kerosene.
More preferably, a process control agent is added in the wet grinding or dry grinding process, wherein the process control agent for dry grinding is one or a combination of methanol, ethanol or stearic acid, and the process control agent for wet grinding is one or a combination of titanate, oleic acid or imidazoline.
Preferably, in (1), the spherical metal matrix powder is one or more of aluminum, copper, magnesium, titanium, iron, nickel and alloy powder thereof.
Preferably, (2) the stirrer is a highly sealed tank with a stirring rod provided with four stirring blades, wherein: the size of a slit between the stirring blade and the tank body is 1-5 mm; the stirring blade rotating at high speed after the stirrer is started generates an annular space in the tank body for mixing powder; the rotating speed range of the stirring rod is 0-10000 rpm.
Preferably, in the step (2), the high-speed stirring and mixing are carried out in a stirrer with a set rotating speed of 1500-10000 rpm; stirring and mixing at a high speed for 3-20 minutes; after the mixing is finished, the shape of the micro-nano flaky metal matrix powder is basically unchanged, and the nano particles are uniformly dispersed on the surface of the micro-nano flaky metal matrix powder.
Preferably, in (2), the nanoparticles are one or more of silicon carbide, titanium carbide, boron nitride, aluminum oxide, silicon oxide, titanium oxide, zirconium oxide, copper oxide and diamond.
Preferably, in the step (2), the protective atmosphere is selected from nitrogen, argon or helium, and is used for preventing the micro-nano flaky metal matrix powder from being oxidized in the processes of high-speed stirring and mixing and mechanical ball milling.
Preferably, in (3), the short-time mechanical ball milling treatment is: under the protective atmosphere, the ball milling treatment time is 30-90 minutes, no process control agent is added in the ball milling process, and under the high-speed impact of ball milling medium balls, the surfaces of the micro-nano flaky metal matrix powder are welded together, so that nano particles are embedded into the micro-nano flaky metal matrix powder to form composite powder.
Preferably, (3) wherein: the characteristic size of the nano particles is between 5 and 300nm, and the total content of the nano particles is 0.1 to 20 wt.%.
More preferably, the total content of the nanoparticles is 0.5-10 wt.%.
Preferably, in (4), the sintering process is atmosphere sintering or vacuum hot pressing sintering, spark ion beam sintering, hot isostatic pressing sintering, and the sintering temperature is higher than the decomposition temperature of the process control agent added in the ball milling process but lower than the melting point of the metal matrix.
Preferably, (4) the densification process comprises: cold pressing, cold isostatic pressing, warm pressing, pressureless sintering, hot pressed sintering, hot isostatic pressing, and one or more of subsequent extrusion, forging, upsetting, and rolling processes.
The invention carries out the grain refinement process of the metal matrix and the dispersion process of the nano particles step by step, thereby solving the problems of rapid and uniform dispersion of the nano particles in the metal matrix:
firstly, replacing traditional spherical powder of dozens of microns with micro-nano sheet metal powder as a mixed raw material, wherein the specific surface area of the mixed raw material is 10-30 times that of the spherical metal powder, the large specific surface area is beneficial to uniform dispersion of nano particles on the surface of the mixed raw material, and the grain refinement of a matrix is realized simultaneously in the process of preparing the micro-nano sheet metal powder, and the grain size is 50-500 nm;
secondly, the adopted stirring and mixing method with extremely high rotation speed in the stirrer under the protective atmosphere utilizes strong shearing force generated by the high-speed rotation (1500-10000 rpm) of the stirring blade in a slit (1-5 mm) between the stirring blade and the tank body and mutual extrusion force between different powders to open the nanoclusters and enable the nanoparticles to be uniformly attached to the surface of the micro-nano flaky metal matrix powder, so that the nanoparticles are dispersed on the surface of the micro-nano flaky metal matrix powder within extremely short time (3-10 minutes), the structural damage to a nano reinforcement body is small, and the dispersion degree is increased along with the increase of the specific surface area of the spherical metal matrix powder. The method is different from the traditional mechanical alloying method, the grain refining process of the matrix alloy and the dispersion process of the nano particles in the traditional mechanical alloying method are carried out synchronously, the variation process of the metal powder in the ball milling process is a repeated large deformation process of flaking, fragmentation, welding, repurposing and repurposing, the nano particles are aggregated on the surface of the metal powder due to the easy aggregation of the nano particles and the small surface area for dispersion after the nano particles and the matrix powder are simply mixed, the nano particles are fused into the matrix powder in the form of clusters along with the ball milling, the dispersion of the nano particles is improved by long-time ball milling, namely the repeated large deformation process of the matrix metal powder, and the dispersion of the nano particles is in direct proportion to the ball milling time and the rotating speed (the longer the time and the higher the rotating speed, the better the dispersibility), therefore, the preparation method provided by the invention effectively shortens the time for uniformly dispersing the nano particles;
and finally, embedding the nano particles into the micro-nano sheet metal matrix powder by adopting short-time (30-90 minutes) mechanical ball milling treatment to promote the interface combination of the nano particles and the micro-nano sheet metal matrix powder, and then obtaining the ultrafine crystal metal matrix composite material with uniformly dispersed nano particles through the subsequent densification process.
The size of the nano reinforcement particles is between 5 and 300nm, the grain size of the metal matrix is only hundreds of nanometers, and the uniform dispersion of the nano particles improves the processing and hardening capacity of the superfine crystal matrix, so that good plasticity is kept under the condition of fully exerting the double mechanisms of superfine crystal strengthening and nano particle strengthening.
In the invention, the superfine crystal means that the size of the final crystal grain is between 100 and 1000 nm.
The mass fraction of the nano particles used as the reinforcement of the nano particle reinforced ultrafine grained metal matrix composite material can be randomly regulated and controlled within the range of 0.1-20 wt.% according to the design requirement. The room temperature strength of the metal matrix composite material prepared by the invention is more than 300MPa, and the elongation is more than 8%.
Compared with the prior art, the invention has the following beneficial effects:
(1) the uniform mixing of the nano particles and the metal matrix can be realized only in a very short time, and the dispersion uniformity is high;
(2) the whole preparation process consists of three parts, namely, micro-nano flaky metal powder preparation by short-time ball milling, short-time high-speed stirring and mixing and short-time mechanical ball milling treatment, the grain refinement process of a metal matrix is separated from the dispersion process of nano particles, and compared with the traditional high-energy ball milling and mixing process, the whole process is energy-saving, time-saving and cost-reducing;
(3) finally, the metal matrix composite material of the ultrafine grain matrix with uniformly dispersed nano reinforced particles not only can exert a composite reinforcement and ultrafine grain reinforcement dual reinforcement mechanism, but also improves the processing and hardening capacity of the ultrafine grain matrix by uniformly dispersing the nano particles in the ultrafine grains, thereby obtaining high strength and high modulus and simultaneously keeping good plasticity;
(4) the preparation method has wide application range, can prepare large-block composite materials, and is suitable for large-scale production.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic flow chart of a method according to an embodiment of the present invention;
FIG. 2 is an SEM photograph of the flake aluminum powder with a thickness of 1-2 μm according to an embodiment of the present invention; wherein: (a) the photograph of the diameter direction of the aluminum flake powder is shown, and the photograph of the thickness direction of the aluminum flake powder is shown;
FIG. 3 is an SEM photograph of nano-sized silicon carbide particles with a size of 50nm according to an embodiment of the present invention;
FIG. 4 is a diagram illustrating a SiC/Al mixed powder after high-speed stirring and mixing in an embodiment of the present invention, wherein: (a) the photograph of the mixed powder is shown, and (b) the photograph of the mixed powder is partially enlarged;
FIG. 5 is a diagram illustrating composite particles formed by mechanically ball milling composite powders for a short time, according to an embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The metal powders used in the following examples were all spray formed and had a purity of greater than 99%, with the remaining chemicals being analytical grade. All the examples are carried out according to the process flow shown in FIG. 1, the room-temperature mechanical properties of the materials in all the examples are carried out according to GB/T228.1-2010, and the stretching rate is 0.5 mm/min.
Example 1: nano silicon carbide/aluminum (SiC/Al) composite material
As shown in fig. 1, a powder metallurgy preparation method of a nano-particle reinforced ultra-fine grained metal matrix composite material, which is used for preparing a nano silicon carbide/aluminum (SiC/Al) composite material, comprises the following steps:
putting 1000g of 10-micron pure aluminum (Al) powder into a stirring ball mill, adding 40g of titanate as a ball milling process control agent by taking absolute ethyl alcohol as a solvent, wherein the ball-material ratio is 20: 1, ball-milling for 1 hour at a rotating speed of 352 r/min, filtering, and drying in vacuum to obtain flaky aluminum powder, wherein the flaky aluminum powder has a diameter of 20-40 mu m, a thickness of 1-2 mu m and a diameter-thickness ratio of 20-40;
taking 100g of nano silicon carbide (SiC) particles, wherein the average particle size is 50nm, adding the particles into absolute ethyl alcohol, and carrying out ultrasonic cleaning, filtering and drying;
adding 950g of the flaky aluminum powder and 50g of nano silicon carbide particles (the volume fraction of SiC is 4.2%) into a stirrer, introducing nitrogen as protective atmosphere, and taking out after running for 5 minutes at the rotating speed of 1750 r/min; adding the mixed powder into a planetary ball mill, and using a 6mm stainless steel ball as a ball milling medium, wherein the ball-material ratio is 10: 1, grinding the mixture for 60 minutes at a rotating speed of 426 revolutions per minute by a ball mill, taking out the composite powder, and cold-pressing the composite powder into a blank with the diameter of 80mm under the pressure of 200 MPa; and then the green body is sintered for 3 hours in a vacuum hot pressing mode at 580 ℃, and then the green body is heated in a vacuum extrusion furnace at 440 ℃ for 1 hour and then is sintered in a vacuum hot pressing mode at a temperature of 25: an extrusion ratio of 1 and an extrusion rate of 2mm/min were extruded into round bars having a diameter of 10 mm.
As shown in FIG. 2, it is an SEM photograph of the flake aluminum powder with a thickness of 1-2 μm, wherein (a) shows that the flake aluminum powder has a complete surface structure and a diameter of 10-50 μm, and (b) shows that the flake aluminum powder has a uniform thickness of 1-2 μm.
As shown in fig. 3, which is an SEM photograph of nano silicon carbide particles having a size of 50nm, the nano silicon carbide particles are agglomerated due to the small particle size.
As shown in fig. 4, which is an SEM photograph of the SiC/Al mixed powder after high-speed precision mixing, it can be seen from (b) of fig. 4 that the nano silicon carbide particles are very uniformly dispersed on the surface of the aluminum flake after mixing, and the aluminum flake maintains its original flake shape (as shown in (a) of fig. 4).
As shown in fig. 5, for the composite particles of 200-400 μm level formed after high energy ball milling for 60 minutes, it can be seen from the particle surface enlarged in fig. 5b that there is substantially no nano silicon carbide particles on the surface, and it can be seen that the nano silicon carbide particles are indeed embedded into the aluminum matrix by short time ball milling; the room temperature mechanical properties of the finally prepared composite are listed in table 1.
Comparative example 1:
950g and 50g of spherical aluminum powder and nano silicon carbide powder which are the same as those in example 1 are taken and directly placed in a planetary ball mill, 2 wt.% of stearic acid is added, and the mixture is ball-milled for 6 hours at 426 revolutions per minute under the protection of argon gas, so that composite powder is prepared. The powder was subjected to compacting, sintering and subsequent deformation and heat treatment in the same process as in example 1, and the room temperature mechanical properties thereof are shown in table 1.
Example 2: nano boron carbide/magnesium composite material
As shown in fig. 1, a powder metallurgy preparation method of a nanoparticle reinforced ultrafine grained metal matrix composite material is used for preparing a nano boron carbide/magnesium composite material, and comprises the following steps:
putting 200g of spherical magnesium powder with the particle size of 30 microns into a stirring ball mill, taking argon as protective atmosphere, adding 6g of stearic acid as a ball milling process control agent, wherein the ball-material ratio is 20: 1, ball-milling for 3 hours at a rotating speed of 423 rpm to obtain flaky aluminum powder, wherein the flake diameter of the flaky aluminum powder is 50-70 mu m, the average flake thickness is 200nm, and the diameter-thickness ratio is more than 200;
nanoborocarbide (B) was prepared according to the method of example 14C) Powder, the average size of the nanometer boron carbide particles is 40 nm;
adding 186g of flaky magnesium powder and 14g of nano boron carbide powder (the volume fraction of boron carbide is 7.5 vol.%) into a high-speed stirring mixer, and taking out after the operation is carried out for 7 minutes at the rotating speed of 1850 revolutions per minute; adding the mixed powder into a planetary ball mill, and using a 6mm stainless steel ball as a ball milling medium, wherein the ball-material ratio is 10: 1, grinding the mixture for 90 minutes at a rotating speed of 426 revolutions per minute by a ball mill, taking out the composite powder, and pressing the composite powder into a blank with the diameter of 40mm at the pressure of 200MPa and the temperature of 150 ℃; and then the green body is sintered by hot pressing at 580 ℃ for 3 hours, and then is heated in a vacuum extrusion furnace at 350 ℃ for 1 hour, and then the temperature is controlled in a range of 25: extruding into a round bar with the diameter of 8mm at an extrusion ratio of 1 and an extrusion rate of 2 mm/min; the room temperature mechanical properties of the finally prepared composite are listed in table 1.
EXAMPLE 3 Nano titanium carbide/titanium composite
As shown in fig. 1, a powder metallurgy preparation method of a nanoparticle reinforced ultrafine grained metal matrix composite material is used for preparing a nano titanium carbide/titanium composite material, and comprises the following steps:
respectively placing 500g of titanium powder with the average particle size of 45 mu m in two planetary ball milling tanks, taking argon as protective atmosphere, respectively adding 2.5g of stearic acid as a ball milling process control agent, wherein the ball-material ratio is 20: 1, ball-milling for 2 hours at a rotating speed of 426 revolutions per minute to obtain flaky titanium powder, wherein the sheet diameter of the flaky titanium powder is 50-70 mu m, the average sheet thickness is 300nm, and the ratio of the sheet diameter to the sheet thickness is more than 150;
485g of the flaky titanium powder and 15g of nano titanium carbide particles with the average diameter of 10nm are added into a stirrer, argon is introduced to serve as protective atmosphere, and the flaky titanium powder is taken out after being operated for 10 minutes at the rotating speed of 2500 r/min; adding the obtained mixed powder into a planetary ball mill, and performing ball-milling on a 10mm stainless steel ball serving as a ball-milling medium according to a ball-material ratio of 20: 1, grinding the mixture for 30 minutes at a rotating speed of 500 r/min by a ball mill, taking out the composite powder, and carrying out hot-pressing sintering at 1100 ℃ for 3 hours under the pressure of 500MPa to prepare a blank with the diameter of 40 mm; and then rolling at 600 ℃, wherein the rolling reduction is 5% for each time and is divided into 10 passes of rolling, the total rolling reduction is 50%, and the room-temperature mechanical properties of the finally prepared composite material are listed in table 1.
Example 4: nano titanium oxide/aluminium alloy composite material
As shown in fig. 1, a powder metallurgy preparation method of a nano-particle reinforced ultra-fine grained metal matrix composite material, which is used for preparing a nano titanium oxide/aluminum alloy composite material, comprises the following steps:
500g of spherical 6061 aluminum (6061Al) alloy powder with the particle size of 30 μm is put into a stirring ball mill, argon is used as protective atmosphere, 5g of stearic acid is added as a ball milling process control agent, and the ball-to-material ratio is 20: 1, ball milling for 3 hours at the rotating speed of 423 rpm to obtain the flaky aluminum powder, wherein the flake diameter of the flaky aluminum powder is 50-70 mu m, the average flake thickness is 200nm, and the diameter-thickness ratio is more than 200.
Taking 25g of titanium oxide powder with the average particle size of 20nm, adding the titanium oxide powder and 475g of flaky aluminum powder into a stirrer, introducing argon gas as protective atmosphere, and taking out the titanium oxide powder after running for 10 minutes at the rotating speed of 2500 rpm; adding the obtained mixed powder into a planetary ball mill, and taking a 6mm stainless steel ball as a ball milling medium, wherein the ball-material ratio is 10: 1, grinding the mixture for 60 minutes at a rotating speed of 426 revolutions per minute by a ball mill, taking out the composite powder, and cold-pressing the composite powder into a blank body with the diameter of 80mm under the pressure of 300 MPa; then, hot-pressing and sintering the blank at 600 ℃ for 3 hours, then preserving the heat in a vacuum extrusion furnace at 530 ℃ for 1 hour, and extruding the blank into a round rod with the diameter of 8mm at the extrusion ratio of 25:1 and the extrusion rate of 12 mm/min; then the round bar is heat preserved at 530 ℃ for 2h, then quenched and aged at 180 ℃ for 18h to obtain the final block ultra-fine grain composite material, and the room temperature mechanical properties of the composite material are listed in Table 1.
Example 5: nano alumina/copper composite material
As shown in fig. 1, a powder metallurgy preparation method of a nano-particle reinforced ultra-fine grained metal matrix composite is used for preparing a nano alumina/copper composite, and comprises the following steps:
placing 500g of 30-micron pure copper powder in a stirring ball mill, taking absolute ethyl alcohol as a solvent, adding 2g of titanate as a ball milling control agent, wherein the ball-material ratio is 20: 1, ball milling for 3h at the rotating speed of 352 r/min, filtering, and drying in vacuum to obtain flake copper powder, wherein the flake diameter of the copper powder is 40 +/-3 mu m, and the flake thickness is 500 +/-20 nm.
Taking 50g of alumina powder with the average grain diameter of 10nm, adding the alumina powder and 450g of flaky copper powder into a stirrer together, introducing argon as protective atmosphere, and taking out after rotating at the rotating speed of 3000 r/min for 12 minutes; adding the obtained mixed powder into a planetary ball mill, and using 10mm stainless steel balls as a ball milling medium, wherein the ball-material ratio is 15: 1, grinding the mixture for 90 minutes at a rotating speed of 400 r/min by a ball mill, taking out the composite powder, carrying out cold press molding under 500MPa, sintering the composite powder for 4 hours at 950 ℃ in an argon atmosphere, and repeatedly forging and pressing the sintered composite powder at 800 ℃ to obtain the block nano aluminum oxide/copper composite material, wherein the room-temperature mechanical properties of the composite material are shown in Table 1.
TABLE 1 alloy composition and mechanical properties at room temperature
As can be seen from Table 1, in comparison with comparative example 1, in example 1, the tensile strength and modulus of the composite material are both obviously improved, which indicates that the reinforcing efficiency of SiC is obviously improved, and meanwhile, good plasticity is maintained, the elongation reaches 12%, and the comprehensive mechanical properties are obviously improved.
According to the invention, nanoparticles and micro-nano flaky metal matrix powder are stirred and mixed at a high speed in a stirrer in a protective atmosphere for a short time, and the nanoparticles are uniformly dispersed on the surface of the flaky metal powder by using high shearing force and compression force generated between a stirring rod and a tank body; and further embedding nano metal particles into a metal matrix through high-energy ball milling for a short time to obtain nano particle reinforced metal composite particles, and then obtaining the ultrafine grained metal matrix composite material with uniformly dispersed nano particles through compression molding, sintering and hot extrusion deformation. The composite material prepared by the method has the characteristics of fine metal matrix grains and uniform nano-particle dispersion, and the uniform nano-particle dispersion has a good effect on improving the work hardening capacity of an ultrafine crystal matrix, so that fine grain strengthening and composite strengthening can be fully exerted, good plasticity is kept, and the comprehensive mechanical property is obviously improved compared with that of conventional powder metallurgy. The method of the invention saves time and energy, improves the comprehensive mechanical property of the superfine crystal composite material while reducing the preparation cost, can be used for preparing large materials, and has huge scale application potential.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (12)
1. A powder metallurgy preparation method of a nanoparticle reinforced ultrafine grained metal matrix composite, characterized by comprising the following steps:
(1) ball-milling the spherical metal matrix powder to obtain micro-nano flaky metal matrix powder with a large specific surface area, and simultaneously reducing the grain size of the metal matrix to an ultra-fine grain range;
(2) adding the micro-nano flaky metal matrix powder obtained in the step (1) and nano particles into a stirrer according to a design proportion, and uniformly dispersing the nano particles on the surface of the micro-nano flaky metal matrix powder by high-speed stirring and mixing under a protective atmosphere to obtain mixed powder with uniformly dispersed nano particles;
(3) performing short-time mechanical ball milling treatment on the mixed powder obtained in the step (2) to enable nano particles to be embedded into micro-nano flaky metal matrix powder, so as to obtain composite powder with uniformly dispersed nano particles;
(4) and (4) performing pressing, blank forming, sintering and densification treatment on the composite powder obtained in the step (3) to obtain the nano-particle reinforced superfine crystal metal matrix composite material.
2. The powder metallurgy method for preparing nano-particle reinforced ultra-fine grained metal matrix composite according to claim 1, wherein in the step (1): the diameter of the spherical metal matrix powder is between 1 and 100 mu m; the grain size of the micro-nano flaky metal matrix powder obtained after ball milling is 50-500 nm, the specific surface area is 10-30 times of that of the original spherical metal matrix powder, the thickness is 0.1-2 mu m, and the sheet diameter is 5-500 mu m.
3. The powder metallurgy method for preparing nano-particle reinforced ultra-fine grained metal matrix composite according to claim 2, wherein the ball milling process is wet milling or dry milling, and the wet milling solvent is one of water, ethanol or kerosene.
4. The powder metallurgy method for preparing nano-particle reinforced ultra-fine grained metal matrix composite according to claim 3, wherein a process control agent is added during wet grinding or dry grinding, the process control agent during dry grinding is selected from one or a combination of methanol, ethanol or stearic acid, and the process control agent during wet grinding is selected from one or a combination of titanate, oleic acid or imidazoline.
5. The powder metallurgy method for preparing nano-particle reinforced ultra-fine grained metal matrix composite according to any one of claims 1 to 4, wherein the spherical metal matrix powder is one or more of aluminum, copper, magnesium, titanium, iron, nickel and alloy powder thereof.
6. The powder metallurgy method for preparing nano-particle reinforced ultrafine grained metal matrix composite according to claim 1, wherein the high speed stirring and mixing is performed in a stirrer with a set rotation speed of 1500 to 10000 rpm, and the time of the high speed stirring and mixing is 3 to 20 minutes; after the mixing is finished, the shape of the micro-nano flaky metal matrix powder is basically unchanged, and the nano particles are uniformly dispersed on the surface of the micro-nano flaky metal matrix powder.
7. The powder metallurgy method for preparing nano-particle reinforced ultra-fine grained metal matrix composite according to claim 6, wherein the stirrer is a high-sealed tank having a stirring rod with four stirring blades, wherein: the size of a slit between the stirring blade and the tank body is 1-5 mm; after the stirrer is started, the stirring blade rotating at a high speed generates an annular space in the tank body for mixing powder; the rotating speed range of the stirring rod is 0-10000 rpm.
8. The powder metallurgy method for preparing nano-particle reinforced ultra-fine grained metal matrix composite according to claim 1, wherein the nano-particles are one or more of silicon carbide, titanium carbide, boron nitride, aluminum oxide, silicon oxide, titanium oxide, zirconium oxide, copper oxide, and diamond.
9. The powder metallurgy method for preparing nano-particle reinforced ultra-fine grained metal matrix composite according to any one of claims 6 to 8, wherein the protective atmosphere is one of nitrogen, argon or helium.
10. The powder metallurgy method for preparing nano-particle reinforced ultra-fine grained metal matrix composite according to claim 9, wherein the sintering process is atmosphere sintering or vacuum hot pressing sintering, spark ion beam sintering, hot isostatic pressing sintering, and the sintering temperature is higher than the decomposition temperature of a process control agent added in the ball milling process but lower than the melting point of the metal matrix; the densification treatment comprises the following steps: cold pressing, cold isostatic pressing, warm pressing, pressureless sintering, hot pressed sintering, hot isostatic pressing, and one or more of subsequent extrusion, forging, upsetting, and rolling processes.
11. The powder metallurgy preparation method of nano-particle reinforced ultra-fine grained metal matrix composite according to claim 1, wherein the short time mechanical ball milling treatment is: under the protective atmosphere, the ball milling treatment time is 30-90 minutes, no process control agent is added in the ball milling process, and under the high-speed impact of ball milling medium balls, the surfaces of the micro-nano flaky metal matrix powder are welded together, so that nano particles are embedded into the micro-nano flaky metal matrix powder to form composite powder.
12. The powder metallurgy method for preparing nano-particle reinforced ultra-fine grained metal matrix composite according to claim 1 or 11, wherein the composite powder comprises: the characteristic size of the nano particles is between 5 and 300nm, and the total content of the nano particles is 0.1 to 20 wt.%.
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