CN108080644B - Powder metallurgy preparation method of high-strength toughened metal-based composite material - Google Patents
Powder metallurgy preparation method of high-strength toughened metal-based composite material Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention discloses a powder metallurgy preparation method of a high-toughness metal-based composite material, belonging to the field of metal-based composite materials. The method comprises the following steps: (1) performing ball milling treatment on the mixed powder of the metal powder and part of the reinforcing phase; stopping ball milling until all crystal grains in the metal powder reach superfine grains; (2) adding the rest reinforcing phase into the powder subjected to ball milling in the step (1), and continuing ball milling until the reinforcing phase is completely dispersed; (3) and (3) treating the powder subjected to ball milling in the step (2) by adopting a powder metallurgy sintering process to obtain the high-strength and high-toughness metal-based composite material. The invention adds the reinforced phase step by step, so that the reinforced phase is distributed in the matrix orderly. The grain refinement function of the reinforced relative matrix is utilized to regulate and control the grain distribution to form a coarse and fine grain gradient hierarchical structure, thereby realizing the strengthening and toughening of the material. The method not only can simplify the process flow, but also can improve the strong plasticity of the material.
Description
Technical Field
The invention relates to the technical field of metal-based composite materials, in particular to a powder metallurgy preparation method of a high-strength and high-toughness metal-based composite material.
Background
The metal-based composite material is a solid phase material formed by taking metal or alloy as a continuous phase and adding high-performance reinforcing phases such as ceramic particles, fibers, carbon nanotubes and the like into the continuous phase, and has the characteristics of high strength, high modulus, wear resistance, fatigue resistance and the like. Has wide application prospect in the fields of aerospace, nuclear industry, transportation and national defense.
When the crystal grains of the matrix alloy are ultra-fine grains, the strength of the metal matrix composite material is greatly improved, but the strength is greatly reduced at the cost of great loss of material plasticity. Especially when nanoparticles or the like are used as the reinforcing phase, they have a better reinforcing effect (N. Chawla et al, Mechanical behavor of particulate recycled metallic matrix composites, Advanced Engineering Materials, 2001, volume 3, page 357-. However, the conventional metallurgical technology method is difficult to uniformly disperse the nano-reinforcing phase in the matrix, and the cost and the productivity of the nano-reinforcing metal matrix composite material synthesized by adopting a chemical or physical method are difficult to meet the requirements of industrial application. Therefore, the high-energy ball milling method becomes the main method for dispersing the nano reinforcing phase, but the high-energy ball milling can form a large amount of ultra-fine crystals and even nano crystals in the matrix. Although the strength of the material is improved, the elongation of the material is sharply reduced or even disappears due to the lower dislocation holding capacity of the ultra-fine grain and nano-grain structures. In addition, the ultra-fine grain structure composite material has the phenomenon of strength reduction caused by premature local deformation of the material due to insufficient deformation coordination capability (I.Mobashereporur et Al, Effect of nano-size Al)2O3The relationship of the mechanical fibers of the synthesis 7075 inorganic alloys by mechanical alloys, Materials Chemistry and Physics, 2013, Vol. 138, p. 535 and 541).
For this reason, a concept of a hierarchical structure was introduced, in which coarse-grained aluminum powder without ball milling was mechanically mixed into a composite powder after ball milling, and an attempt was made to improve the elongation of the material by using the dislocation-holding capacity and deformation-coordinating capacity of coarse grains (R.G.Vogt, etc., Cryomilled aluminum alloy and boron carbide nano-composite plate, Journal of Materials Processing Technology, 2009, volume 209, page 5046-5053; Z.Zhang, etc., Mechanical behavor of ultra-grained Al composites recycled with B4C nanoparticles, script material, 2011, volume 65, page 652-655), but the obtained effect was limited, and the limited elongation was obtained at the expense of a certain strength loss. The reason for this is that the size difference between the ultra-fine grain and the coarse grain is too large, and the reinforcing phase is completely distributed in the matrix of the ultra-fine grain structure, stress concentration is formed prematurely in the ultra-fine grain region during deformation, while the relaxation effect of the randomly distributed coarse grains on the stress concentration and the ability to prevent crack propagation are limited, and it is difficult to prevent instability caused by local deformation. In addition, the step of adding coarse powder increases the process flow, which is not beneficial to high-efficiency preparation.
Disclosure of Invention
The invention aims to provide a powder metallurgy preparation method of a high-strength and high-toughness metal-based composite material, which can effectively improve the performance and preparation efficiency of the material and is suitable for various reinforcing phases and matrixes.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a powder metallurgy preparation method of a high-strength toughened metal-based composite material comprises the following steps:
(1) performing ball milling treatment on the mixed powder of the metal powder and part of the reinforcing phase; stopping ball milling until all crystal grains in the metal powder reach superfine grains, wherein the powder is obviously deformed and welded;
(2) adding the rest reinforcing phase into the powder subjected to ball milling in the step (1), continuing ball milling until the reinforcing phase agglomeration disappears, and stopping ball milling;
(3) and (3) treating the powder subjected to ball milling in the step (2) by adopting a powder metallurgy sintering process and carrying out plastic processing to obtain the high-strength and high-toughness metal-based composite material.
In the step (1), the metal powder is Al, Al alloy, Cu alloy, Ni-based alloy, Fe, or Fe-based alloy.
In the step (1), the reinforcing phase is SiC or Al2O3、B4C、TiB2、TiC、TiAl、Ti3SiC2WC, AlN, ZrC, VC, carbon nanotubesAnd one or more of graphene.
In the composite material, when the used reinforcing phase is particles with the size of more than or equal to 300nm, the volume content of the reinforcing phase is 3-40%, and preferably 15-30%; when the used reinforcing phase is particles with the size less than 300nm, the volume content of the reinforcing phase is 0.5-15%, preferably 2-10%; when the used reinforcing phase is carbon nano tube or graphene, the volume content of the reinforcing phase is 0.5-15%, preferably 2-10%.
In the step (1), the added part of the reinforcing phase accounts for 0-50%, preferably 10-30% of the total reinforcing phase; in the ball milling process, the rotating speed is 50-250 rpm/min, and the ball material weight ratio is (10-30): 1.
when the ball milling in the step (1) is stopped, more than 50% of the crystal grains in the metal powder are micron-sized crystal grains, and if superfine grains exist, the size of the superfine grains is not less than 150 nm.
In the step (2), when the rest of the reinforcing phase is added, the process is carried out for one time or multiple times; and after the reinforcing phase is added for the last time, ball milling is stopped until the agglomeration of the reinforcing phase disappears.
In the step (2), when the residual reinforcing phase is added, the addition is completed 1 to 10 times, preferably 1 to 3 times; in the ball milling process in the step (2), the rotating speed is 50-400 rpm, and the ball material weight ratio is 10: 1-30: 1.
In the step (3), the powder metallurgy sintering process is hot pressing sintering, cold isostatic pressing, hot isostatic pressing, extrusion or spark ion beam sintering under the atmosphere or vacuum condition, and the sintering temperature is higher than the decomposition temperature of the control agent in the ball milling process.
In the step (3), the plastic working is one or more of forging, rolling or extrusion so as to meet the requirements of the size, the shape and the performance of the material at the later stage.
The invention has the following advantages and beneficial effects:
1. the invention provides a simple, convenient and novel ball milling method for preparing a high-toughness metal-based composite material, which is characterized in that a reinforcing phase is added in stages for ball milling, the distribution of the reinforcing phase is regulated and controlled, and a coarse crystal area and a coarse and fine crystal gradient transition structure which are distributed in a net shape are formed by utilizing the refining effect of reinforcing relative crystal grains, so that the deformation coordination of the material is improved, and the toughness of the material is realized.
2. The invention adds the reinforcing phase by times, so that the reinforcing phase is orderly distributed in the matrix to form a depletion region of partial reinforcing phase and the depletion region is kept until the ball milling is finished. Because the reinforcing phase has pinning and refining effects relative to the matrix grains, in the final material, the reserved reinforcing phase depleted area is weaker due to the less pinning effect of the reinforcing phase to form a coarse crystal area. Because there is no distinct boundary between the coarse and fine grains, there is no distinct boundary between coarse and fine grains, i.e., there is no abrupt change in adjacent grain sizes and the coarse and fine grains transition in gradient. Experiments prove that after plastic deformation, coarse crystals are distributed in an ordered net shape, so that an optimized hierarchical structure is formed. Compared with the prior art, the ordered hierarchical structure can promote deformation coordination, more effectively prevent or weaken local deformation and stress concentration, and inhibit the characteristic of high localization of superfine crystal deformation, thereby postponing deformation instability of the material, simultaneously improving the strength and plasticity of the material, and realizing the strengthening and toughening of the material.
3. The method is suitable for large-scale preparation of high-toughness metal matrix composite, the reinforced phase is not limited, the method is simple, the controllability is good, the preparation cost is low, and the effect is obvious.
4. The invention provides a new process for preparing the composite material by high-energy ball milling, does not need additional process to add coarse-crystal matrix components, does not increase preparation period and cost, and has wide application prospect.
Drawings
FIG. 1 shows coarse crystals in a network distribution and fine crystal regions therebetween in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
For further understanding of the present invention, the following examples are given to illustrate the powder metallurgy method for preparing metal matrix composite materials according to the present invention, and the scope of the present invention is not limited by the following examples.
Example 1
Pure aluminum powder with an average particle size of 13 mu m and 60nm Al are used2O3The particles are used as raw materials to prepare the nano-alumina reinforced aluminum matrix composite material with the mass fraction of 5 percent. The method comprises the following steps:
(1) adding nano alumina particles with the mass fraction of 2 percent (the proportion in the mixed powder) into pure aluminum powder, filling the mixture into a ball milling tank, adding 3 percent (the proportion in the mixed powder) of stearic acid as a process control agent, and ball milling the mixture for 1 hour on a planetary ball mill at 100 revolutions per minute to mix the mixture evenly. The weight ratio of the ball material is 20: 1.
(2) the rotating speed is increased to 300 r/m, and the ball milling is carried out for 2 h.
(3) The nano alumina particles were again added to the ball mill pot in a mass fraction of 3% (the proportion in the mixed powder) and ball milled at 100 rpm for 1 hour to be uniformly mixed. The weight ratio of the ball material is 20: 1.
(4) the rotating speed is increased to 300 r/min, and the ball milling is carried out for 6 h.
(5) Taking out the powder, putting into a die, and cold pressing under the pressure of 20 MPa.
(6) Placing the mold into a vacuum sintering furnace for bidirectional hot pressing, heating to 400 deg.C, maintaining the temperature for 30min to remove stearic acid, heating to 630 deg.C, maintaining the temperature for 1h, and hot pressing at vacuum degree of 10-1～10-2Pa and the pressure is 50 MPa.
(7) And (3) keeping the temperature of the hot pressing ingot at 480 ℃ for 2h for forging, wherein the forging height ratio is 4: 1.
in the embodiment, the reinforcing phase is added step by step and the rotation speed and time of the high-energy ball milling are adjusted, so that the reinforcing phase is macroscopically non-uniformly distributed, a coarse-fine crystal gradient transition structure and a reticular coarse crystal distribution structure (as shown in figure 1) are formed, and the strength and the elongation of the material are simultaneously improved by the hierarchical structure. Microstructure observation shows that the powder obtained in the step (2) is flaky, part of the powder is subjected to cold welding to a certain extent, and the grain size is larger than 2 microns. Coarse grains in aluminum powder clusters formed by cold welding the aluminum powder in the final material are reserved, coarse grain bands with grains of about 2 microns are formed, a coarse grain net is formed after hot pressing, the rest is ultra-fine grains with the grain size of about 200nm, and transition exists between the coarse grains and the fine grains. The mechanical property test shows that the yield strength of the material is 350MPa and is improved by 180 percent relative to a matrix subjected to ball milling for 6h, the tensile strength reaches 403MPa and is improved by 118 percent relative to the matrix, and meanwhile, the elongation is 8 percent. Compared with the uniform 5 percent alumina reinforced aluminum matrix composite material obtained in the common ball milling process, the tensile strength is improved by 23MPa, and the elongation is improved from 2.1 percent to 8 percent. The tensile strength reaches 130MPa at 375 ℃, and is improved by 175 percent compared with a pure aluminum matrix.
Example 2
Pure copper powder with an average particle size of 16 mu m and 60nm Al are used2O3The particles are used as raw materials to prepare the nano-alumina reinforced copper-based composite material with the mass fraction of 3 percent. The method comprises the following steps:
(1) adding 1 mass percent (proportion in mixed powder) of nano alumina particles and 2 percent of stearic acid (proportion in mixed powder) into pure copper powder, filling the mixture into a ball milling tank, and carrying out ball milling on a planetary ball mill for 1 hour at 100 revolutions per minute to mix the mixture evenly. The weight ratio of the ball material is 20: 1.
(2) the rotating speed is increased to 250 r/min, and the ball milling is carried out for 1 h.
(3) The nano alumina particles of 2% by mass (ratio in the mixed powder) were again added to the ball mill pot and ball milled at 100 rpm for 1 hour to be uniformly mixed. The weight ratio of the ball material is 20: 1.
(4) the rotating speed is increased to 280 r/min, and the ball milling is carried out for 5 h.
(5) Taking out the powder, putting into a die, and cold pressing under the pressure of 20 MPa.
(6) Placing the mold into a vacuum sintering furnace for bidirectional hot pressing, heating to 400 deg.C, maintaining the temperature for 30min to remove stearic acid, heating to 1030 deg.C, maintaining the temperature for 2h, and hot pressing at vacuum degree of 10-1～10-2Pa, and the pressure is 55 MPa.
(7) And (3) preserving the heat of the hot-pressed ingot at 800 ℃ for 2h, and extruding the hot-pressed ingot, wherein the deformation ratio is 16: 1.
mechanical property tests along the extrusion direction show that the tensile strength of the material reaches 835MPa, the elongation is 15 percent, and the microhardness reaches 2453 MPa.
Example 3
SiC particles with the average particle size of 75nm and Ti-6Al-4V alloy powder with the particle size of 44 mu m are adopted for preparing and blending to prepare the nano SiC particle reinforced titanium-based composite material with the particle volume content of 6 percent. The method comprises the following steps:
(1) the alloy powder and 3% (in the mixed powder) of SiC particles were charged into a planetary ball mill pot and ball-milled at 100 rpm for 1 hour to be mixed uniformly. The weight ratio of the ball material is 20: 1.
(2) the rotating speed is increased to 220 r/m, and the ball milling is carried out for 1.5 h.
(3) The nano SiC particles of 3% by mass (ratio in the mixed powder) were again added and ball-milled at 100 rpm for 1 hour to mix uniformly. Ball material ratio 20: 1.
(4) the rotating speed is increased to 240 r/m, and the ball milling is carried out for 6 h.
(5) Placing the mold into a vacuum sintering furnace for bidirectional hot pressing, heating to 400 deg.C, maintaining the temperature for 30min to remove stearic acid, heating to 1200 deg.C, maintaining the temperature for 2h, and hot pressing at vacuum degree of 10-1～10-2Pa and a pressure of 65 MPa.
(6) And (3) carrying out heat treatment on the hot-pressed ingot at 900 ℃ for 50min, then carrying out air cooling, heating to 540 ℃, then carrying out heat preservation for 6h, and then quenching.
The composite material is tested by sampling along any direction, the tensile strength reaches 1205MPa, the yield strength reaches 1110MPa, and the elongation is 3-5%.
The above embodiments are merely intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention has been described with reference to preferred embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims.
Claims (6)
1. A powder metallurgy preparation method of a high-strength toughened metal-based composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) performing ball milling treatment on the mixed powder of the metal powder and part of the reinforcing phase; stopping ball milling until all crystal grains in the metal powder reach superfine grains, wherein when ball milling is stopped, more than 50% of the crystal grains in the metal powder are micron-sized crystal grains, and if superfine grains exist, the size of the crystal grains is not less than 150 nm;
(2) adding the rest reinforcing phase into the powder subjected to ball milling in the step (1) for one time or multiple times, continuing ball milling until the reinforcing phase agglomeration disappears, and stopping ball milling;
(3) processing the powder subjected to ball milling in the step (2) by adopting a powder metallurgy sintering process and performing plastic processing to obtain the high-strength and high-toughness metal-based composite material;
in the composite material, when the used reinforcing phase is particles with the size of more than or equal to 300nm, the volume content of the reinforcing phase is 15-30%; when the used reinforcing phase is particles with the size smaller than 300nm, the volume content of the reinforcing phase is 2-10%; when the used reinforcing phase is a carbon nano tube or graphene, the volume content of the reinforcing phase is 2-10%;
in the step (1), the added part of the reinforcing phase accounts for 10-30% of the whole reinforcing phase; in the ball milling process, the rotating speed is 50-250 rpm/min, and the ball material weight ratio is (10-30): 1.
2. the powder metallurgy preparation method of the high-toughness metal-matrix composite material according to claim 1, is characterized in that: in the step (1), the metal powder is Al, Al alloy, Cu alloy, Ni-based alloy, Fe or Fe-based alloy.
3. The powder metallurgy preparation method of the high-toughness metal-matrix composite material according to claim 1, is characterized in that: in the step (1), the reinforcing phase is SiC or Al2O3、B4C、TiB2、TiC、TiAl、Ti3SiC2One or more of WC, AlN, ZrC, VC, carbon nanotubes and graphene.
4. The powder metallurgy preparation method of the high-toughness metal-matrix composite material according to claim 1, is characterized in that: in the step (2), when the residual enhancement phase is added, the addition is finished for 1-10 times; in the ball milling process in the step (2), the rotating speed is 50-400 rpm, and the ball material weight ratio is 10: 1-30: 1.
5. The powder metallurgy preparation method of the high-toughness metal-matrix composite material according to claim 1, is characterized in that: in the step (3), the powder metallurgy sintering process is hot pressing sintering, cold isostatic pressing, hot isostatic pressing, extrusion or spark ion beam sintering under the atmosphere or vacuum condition, and the sintering temperature is higher than the decomposition temperature of a control agent in the use process of ball milling.
6. The powder metallurgy preparation method of the high-toughness metal-matrix composite material according to claim 1, is characterized in that: in the step (3), the plastic processing is one or more of forging, rolling or extrusion so as to meet the requirements of the size, the shape and the performance of the material at the later stage.
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