CN110257738B - Preparation method of superfine carbon particle reinforced metal matrix composite material - Google Patents
Preparation method of superfine carbon particle reinforced metal matrix composite material Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
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Abstract
The invention relates to a preparation method of an ultrafine carbon particle reinforced metal matrix composite material, belonging to the technical field of composite material preparation. The preparation method comprises the following steps: the method comprises the steps of degumming short carbon fibers, carrying out a proper ball milling process and a proper decarbonization-reduction process on the degummed short carbon fibers and metal powder to obtain metal powder embedded with superfine carbon particles with carbon removed from the surface, and carrying out a traditional mixing-pressing-sintering process on the metal powder as a raw material to obtain the superfine carbon particle reinforced metal-based composite material. The superfine carbon particle structure is similar to carbon fiber, the particle size is fine (1-3 mu m), the particle size distribution is narrow, and the superfine carbon particle reinforced metal matrix composite material is uniformly embedded in metal powder.
Description
Technical Field
The invention relates to a preparation method of an ultrafine carbon particle reinforced metal matrix composite material, belonging to the technical field of composite material preparation.
Background
The carbon fiber reinforced metal matrix composite material has a series of advantages of excellent mechanical property, wear resistance, high temperature resistance, arc ablation resistance, good self-lubricating property and the like, and is widely applied to the fields of machine manufacturing, aerospace and the like as a metal matrix composite material. Especially carbon fiber reinforced copper-based composite material, widely used for manufacturing electric brushes, bearing bushes, sliders, electric shock, integrated circuit heat dissipation plates, pantograph slide plates and the like. However, the carbon fiber has a large amount of active functional groups on the surface, so that the carbon fiber is easy to agglomerate and difficult to disperse in the process of mixing with other metals, and the carbon fiber is unevenly distributed in a matrix.
In response to this problem, researchers have proposed methods of dispersing carbon fibers with a dispersant, plating the surface of the carbon fibers with a metal, and replacing the carbon fibers with carbon fiber powder. However, the metal plating technology has long process flow, complex process period, large equipment investment and complex process, and the phenomena of black core and uneven plating layer are easy to occur in metal plating. Chinese patent CN103201026A discloses a fine carbon fiber dispersion liquid which uniformly disperses and defibrates fine carbon fibers having an extremely high aggregating force and forming aggregates in an organic solvent and forms a stable dispersed state. A fine carbon fiber dispersion liquid in which fine carbon fibers are dispersed in an organic solvent, wherein a polymer dispersant is used, and the size of aggregates of the fine carbon fibers contained in the dispersion liquid is 5 [ mu ] m or less. Chinese patent CN 108103422A discloses a Cu-plated short carbon fiber reinforced Cu-based composite material, which is prepared by powder metallurgy to improve the properties of the Cu-based composite material such as density, hardness, conductivity and the like. Firing at 380 ℃ for 30min is adopted as a better carbon fiber degumming process; compared with ultrasonic dispersion and magnetic stirring, the short carbon fiber has good dispersibility when electric stirring is adopted, and the chemical plating Cu plating layer is uniform and compact. With the increase of the content of the Cu-plated short carbon fibers, the density and the conductivity of the composite material show a trend of decreasing, and the hardness shows a trend of increasing firstly and then decreasing, wherein when the content of the Cu-plated short carbon fibers reaches 12.5%, the hardness value of the Cu-based composite material is the highest; the physical properties of the short carbon fiber Cu-based composite material plated with Cu are superior to those of the short carbon fiber composite material not plated with Cu.
Chinese patent CN103333473A discloses a carbon fiber or carbon fiber powder composite material and a processing technology thereof, which comprises the following components by mass percent: (1) unsaturated polyester resin or epoxy resin is taken as a matrix: 35% -55%; (2) carbon fiber or boron fiber: 2% -20%; (3) micro glass spheres or silicon carbide spheres: 5% -15%; (4) 35% -55% of carbon fiber powder; (5) copper powder or copper alloy powder: 2 to 20 percent. The carbon fiber or carbon fiber powder composite material provided by the invention has high specific strength and specific modulus, and a structural member formed by the composite material has the advantages of low density, fine polishing effect, surface fineness, impact resistance, low resistivity and good conductivity. Chinese patent CN105088421B discloses a method for preparing carbon fiber powder, which mainly solves the problems of high energy consumption and low production efficiency in the prior art, and the method for preparing carbon fiber powder adopted by the present invention comprises the following steps: (1) shearing, grinding and mixing continuous carbon fibers and thermoplastic resin in a molten state to obtain a mixture of carbon fiber-containing powder and the thermoplastic resin; (2) dissolving the thermoplastic resin in the mixture with a good solvent for the thermoplastic resin; (3) the technical scheme for obtaining the carbon fiber powder through solid-liquid separation better solves the technical problem and can be used in the industrial production of the carbon fiber powder. Chinese patent CN 104098081B discloses a preparation process of carbon fiber powder with small length-diameter ratio, which comprises the following steps: A. bundling; B. bonding; C. slicing or grinding; D. dissolving; E. separating; F. and (5) purifying. The invention provides a preparation process of carbon fiber powder with small length-diameter ratio, creates a brand new production process, can produce carbon fiber powder with smaller length-diameter ratio and fineness, further can greatly improve the use effect of the carbon fiber powder, and promotes the development of industries and enterprises. In order to solve the problem of agglomeration of carbon fiber powder, Chinese patent CN 104088132B discloses a carbon fiber powder surface modification method, which comprises the steps of firstly carrying out air firing pretreatment on carbon fiber powder, then immersing the pretreated carbon fiber powder into an oxidizing solution for surface modification, and finally carrying out cleaning treatment on the modified carbon fiber powder to obtain the surface-modified carbon fiber powder.
The modified carbon fiber powder obtained by the method has good solvent wettability and dispersion stability, and has good interface bonding capability when being compounded with a matrix.
Disclosure of Invention
The invention provides a preparation method of a superfine carbon particle reinforced metal matrix composite, the process is simple and convenient, the cost is low, the problems that fine carbon particles similar to carbon fiber structures are uniformly embedded in metal powder, and after the carbon particles are embedded into the metal powder as a raw material, part of carbon is exposed outside the metal particles, so that the diffusion among the metal particles is incomplete, and the sintering is not compact are solved, the prepared metal powder has the performances of high strength, high toughness, corrosion resistance and the like of metal, and the performances of heat conductivity, wear resistance, oxidation resistance and the like of the carbon fibers, and the preparation process is simple and the cost is low.
The invention relates to a preparation method of an ultrafine carbon particle reinforced metal matrix composite material, which comprises the following steps:
step one
According to a set proportion, preparing the degummed short carbon fiber and the matrix metal powder, and then carrying out high-energy ball milling to obtain mixed powder;
the rotating speed of the high-energy ball milling is 220-350 r/min, and the ball milling time is more than or equal to 6 h;
step two
Pre-oxidizing the mixed powder obtained in the first step in an oxygen-containing atmosphere; obtaining powder to be reduced; the temperature of the pre-oxidation treatment is 250-400 ℃, and the treatment time is 10-60min, preferably 20-40 min;
step three
Carrying out reduction annealing treatment on the powder to be reduced obtained in the step two in a reducing atmosphere; the temperature of the reduction annealing treatment is 0.3-0.65 times of the melting point of the base metal, the annealing time is more than or equal to 30min, preferably 30-60 min, and the annealing atmosphere is H2Reducing one or more kinds of reducing atmosphere in CO to obtain metal powder only containing carbon particles inside;
step four
Uniformly mixing the annealed powder with other particle powder, and then carrying out cold pressing forming to obtain a cold pressed blank;
or
Cold-pressing the annealed powder to form a cold-pressed blank;
or
Uniformly mixing the annealed powder with other particle powder, and then carrying out hot press forming to obtain a finished product; when in hot pressing, the temperature is controlled to be 70-85% of the melting point of the matrix metal, and the time is less than or equal to 90 min;
or
Hot-pressing the annealed powder to obtain a finished product; when in hot pressing, the temperature is controlled to be 70-85% of the melting point of the matrix metal, and the time is less than or equal to 90 min;
step five
Sintering the cold pressed compact obtained in the third step in a protective atmosphere or a vacuum atmosphere; obtaining a finished product;
the sintering temperature is 60-80% of the melting point of the base metal, and the heat preservation time is more than or equal to 10min, preferably 10-200 min, and further preferably 0.5-3 h.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; under a protective atmosphere; heating the short carbon fiber bundle to 650-800 ℃, and carrying out heat preservation treatment for 20-90 min; obtaining the degummed short carbon fiber. Preferably, the short carbon fiber bundle has a diameter of 6 to 8 μm and a length of 1 to 4 mm.
The preparation method of the superfine carbon particle reinforced metal matrix composite material is carried out in a protective atmosphere; in the first step, the volume ratio of the degummed short carbon fiber to the matrix metal powder is 2-19: 1 to 3. Preferably 1-16: 1. as further preference; in the first step, the mass percentage of the short carbon fiber in the degummed short carbon fiber and the matrix metal powder is 20-90%.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; under a protective atmosphere; in the first step, according to the mass ratio, grinding balls: (degummed short carbon fiber + matrix metal powder) 1:5 to 8. Preferably 1: 6 to 7.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; the base metal is at least one selected from iron, copper, iron, nickel, chromium, manganese and silver.
Preferably, the particle size of the base metal powder is 30-250 μm; the particle size of the other particle phase powder is 10-400 mu m.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; in the first step, the rotating speed of the high-energy ball milling is 220-350 r/min, and the ball milling time is 6-14 h.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; in the second step, the oxygen-containing atmosphere is preferably air.
In industrial application, the temperature and time of the pre-oxidation stage are strictly controlled; the content of C in the final product and the mechanical properties of the final product are seriously affected.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; in step three, the reducing atmosphere has H2And CO.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; in the fourth step, the powder after the reduction annealing and other particle powder are put into a V-shaped mixer to be stirred uniformly; the stirring speed of the V-shaped mixer is 80-120r/min, and the mixing time is 2-5 h. The other particle powder is selected from at least one of silicon dioxide, granular graphite, flake graphite, hard ceramic, aluminum oxide, silicon carbide, titanium carbide, tungsten carbide and high-entropy alloy; the other particles account for 0-45% of the total mass of the raw materials.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; in the fourth step of the method, the first step of the method,
the pressure of the cold press molding is 200-600 MPa, and the pressure maintaining time is 20-30 s;
the pressure of the hot pressing is 200-600 MPa; the hot pressing temperature is 70-85% of the melting point of the matrix metal, and the heat preservation and pressure maintaining time is 2-90min, preferably 10-30 min.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; in the obtained finished product, the particle size of the carbon particles is 1-3 mu m.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; in the obtained finished product, the mass percentage content of the carbon particles is less than or equal to 20 percent, and preferably 1-20 percent.
The invention relates to a preparation method of a superfine carbon particle reinforced metal matrix composite material; in the obtained finished product, the structure of the ultrafine carbon particles is similar to that of carbon fibers.
The invention relates to a preparation method of a carbon particle reinforced metal matrix composite; the short carbon fiber is degummed. The surface of the existing carbon fiber on the market is coated and solidified with an organic colloid layer, and the surface sizing agent of the carbon fiber is removed through degumming treatment, so that the roughness of the surface of the carbon fiber is increased, the subsequent (grinding) treatment can remove the 'constraint/limitation' of the sizing agent, the impurities on the surface of the carbon fiber are removed, and otherwise, the breakage rate is very low. The invention strictly controls the length of the short carbon fiber as the raw material and needs to be a product after degumming treatment, and aims to be matched with the ball milling rotating speed, the grinding balls and the proportion of the invention, so that the superfine carbon fiber and the embedding in the metal particles can be well realized, and the metal powder embedded with the superfine carbon particles can be obtained by combining the annealing treatment after ball milling.
In the carbon particle reinforced metal matrix composite material designed and prepared by the invention, the particle size of the ultrafine carbon particles is only 1-3 mu m, the particle size distribution is narrow, the purity is high, the structure is complete and is similar to carbon fibers, and therefore, the carbon particle reinforced metal matrix composite material keeps the excellent characteristics of the carbon fibers such as high heat conductivity, high wear resistance, high oxidation resistance and the like.
The invention firstly tries to prepare metal powder embedded with ultrafine carbon particles by adopting short carbon fibers prepared by a degumming treatment process through high-energy ball milling and annealing processes with proper ball milling parameters; on the basis, the carbon particle reinforced metal powder is adopted to replace metal powder as a raw material, and the carbon particle reinforced metal matrix composite material with high performance can be obtained by combining a decarbonization-deoxidation process and pressing-sintering. The prepared composite material has the performances of high strength, high toughness, corrosion resistance and the like of metal, and the performances of heat conductivity, wear resistance, oxidation resistance and the like of carbon fiber, and has the advantages of simple preparation process and low cost. The invention relates to an application of a carbon particle reinforced metal matrix composite material, which comprises the fields of heat conduction materials, conductive materials, friction materials and the like.
Principle and advantages:
selection of short carbon fiber and degumming treatment process. In terms of selection of short carbon fibers, because a large number of active functional groups exist on the surface of carbon fibers, the long carbon fibers are directly used for crushing, and the fibers are easy to agglomerate and cannot be crushed, so that the problem can be avoided by selecting the short carbon fibers. The short carbon fiber treatment method adopts a degumming and ball milling process, because the surface of the carbon fiber sold in the market is coated with a solidified colloid layer, the degumming treatment is needed to remove the sizing agent on the surface of the carbon fiber, so that the subsequent (grinding) treatment can remove the 'constraint/limitation' of the sizing agent, impurities and active functional groups on the surface of the carbon fiber are removed by the degumming process, otherwise, the breakage rate is very low, the ball milling rotation speed, the grinding balls and the proportion are optimized, the ultra-fining of the carbon fiber can be well realized, the metal or alloy powder with the ultra-fine carbon particles similar to the carbon fiber structure and uniformly embedded is obtained, and the problems that the carbon fiber is easy to spontaneously aggregate with the metal powder in the material mixing process and is uniformly distributed in the metal composite material are solved. .
Selection of the surface decarbonization-deoxidation process. The sintering densification of the powder is mainly carried out by the atomic diffusion among the particles, and an oxide film and a heterogeneous phase on the surface of the metal particles become an interface for hindering the sintering, so that the sintering densification among the powder particles is reduced. Although the carbon particles reinforce the metal powder instead of the metal powder can achieve uniform dispersion of carbon in the matrix, the carbon exposed outside the metal powder also hinders sintering diffusion between the metal particles. It is known that carbon is oxidized to form CO at 250-300 ℃ in an aerobic environment2Therefore, the proper short-time oxidation process is selected to remove the carbon on the surface of the metal powder, thereby being beneficial to the subsequent sintering of the metal particles. The short-time low-temperature treatment in an aerobic environment can remove carbon on the surface of metal, but can oxidize copper, nickel, silver and other matrix metals to a certain degree, so that the reduction treatment of metal powder is carried out after the carbon removal process in order to reduce the part of metal, not only can remove an oxidation film of the metal powder, but also can eliminate impurities on the surface of the metal powder and structural defects, so that the subsequent pressing and sintering of the powder are facilitated, and the superfine carbon particles which are complete in structure and approximate to carbon fibers are obtained.
The preparation process is simple and low in cost, and the preparation of the metal-based composite material taking the carbon particle reinforced metal powder with the similar carbon fiber structure as the raw material is realized through degumming-ball milling treatment and the regulation and control of the carbon removal and reduction process parameters.
The morphology of the powder obtained by directly carrying out high-energy ball milling on the commercial short carbon fiber is shown in figure 2. The morphology of the powder obtained by high-energy ball milling the short carbon fiber degummed at 1000 ℃ is shown in fig. 3. The morphology of the powder obtained by ball milling the short carbon fiber degummed at 700 ℃ at a rotating speed which is too high (600r/min) or too low (150r/min) is shown in FIG. 4. The morphology, Raman spectrum and particle size distribution of the carbon particle reinforced metal powder prepared by the short carbon fiber 250r/min high-energy ball milling method after 700 ℃ degumming treatment and the annealing treatment at 800 ℃ are respectively shown in figures 5 and 6. The composite material prepared by directly using carbon particle reinforced metal powder as a raw material without any treatment is shown in fig. 7. The composite material prepared by using the carbon particle reinforced metal powder with the surface decarbonized and without subsequent reduction annealing as the raw material is shown in fig. 8. The composite material prepared by subjecting the carbon particle-reinforced metal powder to surface decarburization annealing and reduction annealing is shown in fig. 9.
As shown in fig. 2 to 4, the short carbon fiber is not degummed, or the degummed temperature is too high, or the high-energy ball milling rotation speed is too fast or too slow, or the subsequent annealing treatment is not performed, so that the preparation of the ultrafine carbon particles with the similar carbon fiber structure cannot be realized. As can be seen from fig. 5 to 6, the degumming treatment combined with the appropriate high-energy ball milling process and the subsequent high-temperature annealing process not only realizes the crushing of the short carbon fibers, but also obtains the ultrafine carbon particles having a complete structure and similar to carbon fibers, thereby fully exerting the advantages of the ultrafine carbon particles. However, the surface of the carbon particle-reinforced metal powder is exposed to a large amount of carbon particles, which hinders the subsequent sintering. As can be seen from fig. 7 and 8, the carbon particle-reinforced metal powder is directly used as a raw material without any treatment, or is subjected to only a decarbonization treatment without reduction annealing, and a large number of pores are formed in the mixed material-pressed-sintered composite material due to the obstruction of the carbon interface. As can be seen from fig. 9, the surface decarburization annealing and the reduction annealing process with optimized parameters are adopted to achieve densification of the sintered metal particles, so that the metal matrix composite material with uniformly distributed carbon particles and small porosity is obtained, and the obtained composite material has excellent and uniform performance and good market prospect.
In a word, the invention has the advantages of simple preparation process (only degumming, ball milling, short-time decarburization annealing and deoxidation annealing), low cost, excellent and uniform performance of the obtained carbon particle reinforced metal matrix composite material and good market prospect.
Drawings
FIG. 1 is a flow diagram of one embodiment of a carbon particle reinforced metal matrix composite according to the present invention;
FIG. 2 is a powder SEM morphology obtained by directly subjecting commercially available short carbon fibers to high energy ball milling;
FIG. 3 is a powder SEM appearance obtained by high-energy ball milling short carbon fibers subjected to degumming treatment at 1000 ℃ and electrolytic copper powder;
FIG. 4 shows the SEM morphology of powder obtained by ball milling short carbon fibers degummed at 700 ℃ and electrolytic copper powder at a rotating speed of over-high (600r/min) or over-low (150 r/min);
FIG. 5 shows SEM morphology of powder prepared by high-energy ball milling at 250r/min of short carbon fiber degummed at 700 ℃ and electrolytic copper powder prepared by the invention;
FIG. 6 is a Raman spectrum of powder prepared by a 250r/min high-energy ball milling method of the short carbon fiber degummed at 700 ℃ and the electrolytic copper powder prepared by the invention;
FIG. 7 is a composite material prepared by directly using carbon particle reinforced copper powder prepared by a 250r/min high-energy ball milling method on short carbon fiber degummed at 700 ℃ and electrolytic copper powder as raw materials without any decarbonization and reduction treatment;
FIG. 8 shows a copper-based composite material prepared by subjecting short carbon fibers degummed at 700 ℃ and electrolytic copper powder to a 250r/min high-energy ball milling method to obtain carbon particle-reinforced copper powder, carrying out surface decarburization annealing at 280 ℃ for 15min, then carrying out subsequent reduction annealing, and then carrying out mixing, pressing and sintering;
FIG. 9 shows a copper-based composite material prepared by subjecting short carbon fibers degummed at 700 ℃ and electrolytic copper powder to carbon particle-reinforced copper powder prepared by a 250r/min high-energy ball milling method, surface decarburization annealing at 280 ℃ for 15min and hydrogen reduction annealing at 350 ℃ for 30min, and then mixing, pressing and sintering.
Fig. 1 shows a process for preparing ultrafine carbon particles according to the present invention, which comprises: firstly, degumming short carbon fiber and high-energy ball-milling the degummed carbon fiber, then carrying out decarburization and preoxidation treatment on the surface of carbon particle reinforced metal powder obtained by high-energy ball-milling, then carrying out annealing treatment on the preoxidized powder under the protection of reducing atmosphere so as to reduce an oxide film on the surface of the powder and remove surface defects and impurities, and then carrying out conventional mixing, pressing and sintering treatment to obtain the carbon particle reinforced metal-based composite material.
As can be seen from fig. 2 to 4, the short carbon fiber does not undergo special carbonization treatment, or the carbonization treatment temperature is too high, or the high-energy ball milling rotation speed is too fast or too slow, or the subsequent annealing treatment, and the preparation of the metal composite powder in which the copper particles are embedded in the ultrafine carbon particles having a structure similar to that of the carbon fiber cannot be achieved.
As can be seen from fig. 5, the degumming treatment is combined with a suitable high-energy ball milling process and a subsequent high-temperature annealing process, the original short carbon fiber bundle is broken into particles and embedded into copper particles, the particle size of the carbon particles is about 1-3 μm, and the surface of the carbon particle reinforced metal powder is exposed by a large amount of carbon particles.
As can be seen from fig. 6, raman spectroscopy showed that the particle structure shown in fig. 5 had a low degree of orientation, and similar to the carbon fiber structure, the structural defects slightly increased.
As can be seen from fig. 7 to 8, the sintering densification between the metal powder particles cannot be achieved by using the carbon particle-reinforced metal powder as a raw material without any treatment or by using only the decarbonization treatment and without the reduction annealing as a raw material.
As can be seen from fig. 9, the surface decarburization annealing and the reduction annealing process with optimized parameters are adopted to achieve densification of the metal particles by sintering, so that the metal matrix composite material with uniformly distributed carbon particles and small porosity is obtained.
Detailed Description
The technical solutions of the present invention are clearly and completely described below with reference to the drawings of the present invention, and it is obvious that the described embodiments are only some of the technical solutions described in the present invention, but not all of the technical solutions described in the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Comparative example 1
The copper-based composite material prepared in comparative example 1 comprises the following components in percentage by mass:
5.0 percent of short carbon fiber, 1 percent of zirconium carbide and 96 percent of electrolytic copper powder. The particle size of the zirconium carbide was 100 μm, and the particle size of the electrolytic copper powder was 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Directly taking commercially available carbon fibers as objects, adding the commercially available carbon fibers and electrolytic copper powder into ball milling equipment without any pretreatment for high-energy ball milling, wherein the electrolytic copper powder and the short carbon fibers are respectively 80% and 20% by mass percent, the rotating speed is 250r/min, the ball milling time is 6 hours, the ball milled balls are stainless steel balls, and the ball-to-material ratio is 5: 1. The short carbon fibers are not crushed and are adhered to the wall of the ball milling pot, and the appearance of the treated composite powder is shown in figure 2.
Directly mixing the composite powder prepared in a certain proportion and zirconium carbide in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared copper-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the pressed blank is sintered for 2h at 950 ℃, and the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, so that the sample of the comparative example 1 is obtained. The tensile strength of the prepared copper-based composite material is 230 MPa.
Comparative example 2
The copper-based composite material prepared in the comparative example 2 comprises the following components in percentage by mass:
5.0 percent of short carbon fiber, 1 percent of zirconium carbide and 96 percent of electrolytic copper powder. The particle size of the zirconium carbide was 100 μm, and the particle size of the electrolytic copper powder was 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Degumming short carbon fiber at 1000 ℃, adding the degummed short carbon fiber and electrolytic copper powder into ball milling equipment for high-energy ball milling, wherein the electrolytic copper powder and the short carbon fiber are 80% and 20% respectively by mass percent, the rotating speed is 250r/min, the ball milling time is 6h, the ball milled is stainless steel balls, and the ball material ratio is 5: 1. The short carbon fibers are not broken obviously, and the appearance of the treated composite powder is shown in figure 3.
Directly mixing the composite powder prepared in a certain proportion and zirconium carbide in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared copper-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the pressed blank is sintered for 2h at 950 ℃, the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, and the pressure is 0.5MPa, so that the sample of the comparative example 2 is obtained. The tensile strength of the prepared copper-based composite material is 243 MPa.
Comparative example 3
The copper-based composite material prepared in the comparative example 3 comprises the following components in percentage by mass:
5.0 percent of short carbon fiber, 1 percent of zirconium carbide and 96 percent of electrolytic copper powder. The particle size of the zirconium carbide was 100 μm, and the particle size of the electrolytic copper powder was 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Degumming short carbon fiber at 700 ℃, adding the degummed short carbon fiber and electrolytic copper powder into ball milling equipment for high-energy ball milling at the rotating speed of 600r/min for 8h, wherein ball milling balls are stainless steel balls, the ball diameter is 3-10 mm, and the ball-to-material ratio is 6: 1. The short carbon fibers were not significantly broken, most of which were deposited on the top lid of the ball mill pot, and the morphology of the treated composite powder is shown in FIG. 4.
Directly mixing the composite powder prepared in a certain proportion and zirconium carbide in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared copper-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the pressed blank is sintered for 2h at 950 ℃, the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, and the pressure is 0.6MPa, so that the sample of the comparative example 3 is obtained. The tensile strength of the prepared copper-based composite material is 252 MPa.
Comparative example 4
The copper-based composite material prepared in comparative example 4 comprises the following components in percentage by mass:
5.0 percent of short carbon fiber, 1 percent of zirconium carbide and 96 percent of electrolytic copper powder. The particle size of the zirconium carbide was 100 μm, and the particle size of the electrolytic copper powder was 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Degumming the short carbon fiber at 700 ℃ for 60min, adding the degummed short carbon fiber and electrolytic copper powder into ball milling equipment for high-energy ball milling at the rotating speed of 250r/min for 8h, wherein the ball milled is a stainless steel ball, the ball material ratio is 6:1, and the superfine carbon particle embedded copper powder is obtained, and the morphology and the Raman spectrum of the superfine carbon particle embedded copper powder are respectively shown in figures 5-6.
The superfine carbon particles prepared in a certain proportion are directly embedded into copper powder and zirconium carbide to be mixed in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared copper-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the copper-based composite material pressed blank is sintered for 2h at 950 ℃, the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, the pressure is 0.65MPa, and a sample of a comparative example 4 is obtained, wherein the appearance of the sample is shown in figure 7. The porosity is as high as 10%, and the metal particles are not diffused and sintered. The tensile strength of the prepared copper-based composite material is 248 MPa.
Comparative example 5
The copper-based composite material prepared in the comparative example 5 comprises the following components in percentage by mass:
5.0 percent of short carbon fiber, 1 percent of zirconium carbide and 96 percent of electrolytic copper powder. The particle size of the zirconium carbide was 100 μm, and the particle size of the electrolytic copper powder was 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Degumming the short carbon fiber at 700 ℃ for 60min, adding the degummed short carbon fiber and electrolytic copper powder into ball milling equipment for high-energy ball milling at the rotating speed of 250r/min for 8h, wherein the ball milled is a stainless steel ball, and the ball material ratio is 6:1, so as to obtain the superfine carbon particle embedded copper powder. And (3) performing surface decarburization annealing on the carbon particle reinforced copper powder at 280 ℃ for 15min, and then not performing subsequent reduction annealing to obtain carbon particle embedded copper oxide particles with carbon removed on the surfaces.
And embedding the superfine carbon particles prepared in a certain proportion into copper oxide powder and zirconium carbide, and mixing in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared copper-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the copper-based composite material pressed blank is sintered for 2h at 950 ℃, the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, the pressure is 0.55MPa, and a sample of a comparative example 5 is obtained, wherein the appearance of the sample is shown in figure 8. The porosity is 6%, and part of the metal particles are not compact by diffusion sintering. The tensile strength of the prepared copper-based composite material is 265 MPa.
Comparative example 6
The iron-based composite material prepared in comparative example 6 includes the following components in mass percent:
5.0 percent of short carbon fiber, 10 percent of iron-chromium alloy and 40 percent of reduced iron powder. The grain size of the ferrochromium alloy is 100 μm, and the grain size of the reduced iron powder is 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Degumming the short carbon fiber at 700 ℃ for 60min, adding the short carbon fiber and reduced iron powder into ball milling equipment for high-energy ball milling at the rotating speed of 250r/min for 6h, wherein the ball milled is a stainless steel ball, and the ball-to-material ratio is 6:1, so as to obtain the ultrafine carbon particle embedded iron powder. And (3) performing surface decarburization annealing on the carbon particle reinforced iron powder at 350 ℃ for 15min, and then not performing subsequent reduction annealing to obtain carbon particle embedded iron oxide particles with carbon removed on the surfaces.
And embedding the superfine carbon particles prepared in a certain proportion into iron oxide powder and iron-chromium alloy, and mixing in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared iron-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the pressed blank is sintered for 2h at 1050 ℃, the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, and the pressure is 0.45MPa, so that the sample of the comparative example 6 is obtained. The porosity is 12%, and the diffusion sintering between metal particles is not compact. The tensile strength of the prepared iron-based composite material is 380 MPa.
Comparative example 7
The iron-based composite material prepared in comparative example 7 comprises the following components in percentage by mass:
5.0 percent of short carbon fiber, 10 percent of iron-chromium alloy and 40 percent of reduced iron powder. The grain size of the ferrochromium alloy is 100 μm, and the grain size of the reduced iron powder is 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Degumming the short carbon fiber at 700 ℃ for 60min, adding the short carbon fiber and reduced iron powder into ball milling equipment for high-energy ball milling at the rotating speed of 250r/min for 6h, wherein the ball milled is a stainless steel ball, and the ball-to-material ratio is 6:1, so as to obtain the ultrafine carbon particle embedded iron powder. The carbon particle reinforced iron powder is subjected to decarburization annealing at 850 ℃ for 50min and then is subjected to hydrogen reduction annealing at 350 ℃ for 20min, and the obtained carbon particles are embedded into the iron oxide particles and are difficult to reduce due to overhigh oxidation temperature and too long time.
And embedding the superfine carbon particles prepared in a certain proportion into iron powder and iron-chromium alloy, and mixing in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared iron-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the pressed blank is sintered for 2h at 1050 ℃, the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, and the pressure is 0.8MPa, so that the sample of the comparative example 7 is obtained. The porosity is 18%, and the diffusion sintering is not compact because of severe iron oxidation among metal particles. The tensile strength of the prepared iron-based composite material is only 187 MPa.
Comparative example 8
The nickel-based composite material prepared in comparative example 8 comprises the following components in percentage by mass:
10% of short carbon fiber, 5% of aluminum oxide and 85% of electrolytic nickel powder. The particle size of the alumina was 50 μm, the particle size of the carbon particle-embedded copper powder was 120 μm, and the particle size of the electrolytic nickel powder was 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. And degumming the short carbon fiber at 720 ℃ for 60min, adding the short carbon fiber and the electrolytic nickel powder into ball milling equipment for high-energy ball milling at the rotating speed of 250r/min to obtain the superfine carbon particle embedded nickel powder. And (3) performing surface decarburization annealing on the carbon particle reinforced nickel powder at 350 ℃ for 30min, and then not performing subsequent reduction annealing to obtain carbon particle embedded nickel oxide particles with carbon removed on the surfaces.
The carbon particles prepared according to the proportion are embedded into nickel oxide powder and aluminum oxide and mixed in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared nickel-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the pressed blank is sintered for 2h at 1000 ℃, the pressure is 0.8MPa, and the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, so that a sample of a comparative example 8 is obtained. The porosity is 15%, and part of the metal particles are not compact by diffusion sintering. The tensile strength of the prepared nickel-based composite material is 550 MPa.
Example 1
The copper-based composite material prepared in example 1 comprises the following components in percentage by mass:
5.0 percent of short carbon fiber, 1 percent of zirconium carbide and 96 percent of electrolytic copper powder. The particle size of the zirconium carbide was 100 μm, and the particle size of the electrolytic copper powder was 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Degumming the short carbon fiber at 700 ℃ for 60min, adding the degummed short carbon fiber and electrolytic copper powder into ball milling equipment for high-energy ball milling at the rotating speed of 250r/min for 8h, wherein the ball milled is a stainless steel ball, and the ball material ratio is 6:1, so as to obtain the superfine carbon particle embedded copper powder. And (3) performing surface decarbonization annealing on the carbon particle reinforced copper powder at 280 ℃ for 15min, and then performing hydrogen reduction annealing at 350 ℃ for 30min to obtain carbon particle embedded copper particles with carbon removed on the surfaces.
Embedding the superfine carbon particles prepared in a certain proportion into copper powder and zirconium carbide, and mixing in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared copper-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the copper-based composite material pressed blank is sintered for 2h at 950 ℃, the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, the pressure is 0.9MPa, and the sample of the embodiment 1 is obtained, and the appearance of the sample is shown in figure 9. The porosity is 3%, and the diffusion sintering among metal particles is compact. The tensile strength of the prepared copper-based composite material is 450 MPa.
Example 2
The iron-based composite material prepared in example 2 comprises the following components in percentage by mass:
10% of short carbon fiber, 10% of iron-chromium alloy and 80% of reduced iron powder. The grain size of the ferrochromium alloy is 100 μm, and the grain size of the reduced iron powder is 120 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Degumming the short carbon fiber at 750 ℃ for 30min, adding the short carbon fiber and reduced iron powder into ball milling equipment for high-energy ball milling at the rotating speed of 250r/min for 8h, wherein the ball milling ball is a stainless steel ball, and the ball-to-material ratio is 6:1, so as to obtain the ultrafine carbon particle embedded iron powder. Pre-oxidizing carbon particle reinforced iron powder at 350 deg.c for 15 min; then reducing and annealing for 20min at 350 ℃ by hydrogen to obtain the carbon particle embedded iron powder with carbon removed on the surface.
And embedding the superfine carbon particles prepared in a certain proportion into iron powder and iron-chromium alloy, and mixing in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 450MPa, the pressure maintaining time is 20s, the prepared iron-based composite material pressed blank is subjected to pressure sintering under the vacuum protection, the pressed blank is sintered for 2h at 1050 ℃, the pressure is 0.8MPa, and the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, so that the sample of the embodiment 2 is obtained. The porosity is 2.5%, and the diffusion sintering among metal particles is compact. The tensile strength of the prepared iron-based composite material is 746 MPa.
Example 3
The nickel-based composite material prepared in example 3 comprises the following components in percentage by mass:
10% of short carbon fiber, 5% of aluminum oxide and 85% of electrolytic nickel powder. The particle size of the alumina is 40 μm, and the particle size of the electrolytic nickel powder is 150 μm. The short carbon fibers had a diameter of 6 μm and a length of 2 mm. Degumming the short carbon fiber at 700 ℃ for 60min, adding the short carbon fiber and electrolytic nickel powder into ball milling equipment for high-energy ball milling at the rotating speed of 250r/min for 6h, wherein the ball milling ball is a stainless steel ball, and the ball-to-material ratio is 6:1, so as to obtain the ultrafine carbon particle embedded iron powder. Pre-oxidizing the carbon particle reinforced nickel powder at 300 ℃ for 10 min; and then, carrying out hydrogen reduction annealing at 250 ℃ for 30min to obtain the carbon particle embedded nickel powder with carbon removed on the surface.
The superfine carbon particles prepared in a certain proportion are embedded into nickel powder and alumina and mixed in a V-shaped mixer to obtain mixed powder. And then cold pressing is carried out at room temperature, the pressing pressure is 500MPa, the pressure maintaining time is 20s, the prepared nickel-based composite material pressed blank is subjected to pressure sintering under the protection of hydrogen atmosphere, the pressed blank is sintered for 2h at 1000 ℃, the pressure is 0.8MPa, the heating rate and the cooling rate of a furnace are both 10-15 ℃/min, and the pressure is 0.8MPa, so that the sample piece in the embodiment 3 is obtained. The porosity is 2%, and the diffusion sintering among metal particles is compact. The tensile strength of the prepared nickel-based composite material is 1220 MPa.
Claims (10)
1. A method for preparing a superfine carbon particle reinforced metal matrix composite material is characterized in that; the method comprises the following steps:
step one
According to a set proportion, preparing the degummed short carbon fiber and the matrix metal powder, and then carrying out high-energy ball milling to obtain mixed powder;
the rotating speed of the high-energy ball milling is 220-350 r/min, and the ball milling time is more than or equal to 6 h;
step two
Pre-oxidizing the mixed powder obtained in the first step in an oxygen-containing atmosphere; obtaining powder to be reduced; the temperature of the pre-oxidation treatment is 250-400 ℃, and the treatment time is 10-60 min;
step three
Carrying out reduction annealing treatment on the powder to be reduced obtained in the step two in a reducing atmosphere; the temperature of the reduction annealing treatment is 0.3-0.65 times of the melting point of the base metal, and annealing is carried outThe fire time is more than or equal to 30min, and the annealing atmosphere is H2Reducing one or more kinds of reducing atmosphere in CO to obtain metal powder only containing carbon particles inside;
step four
Uniformly mixing the annealed powder with other particle powder, and then carrying out cold pressing forming to obtain a cold pressed blank;
or
Cold-pressing the annealed powder to form a cold-pressed blank;
or
Uniformly mixing the annealed powder with other particle powder, and then carrying out hot press forming to obtain a finished product; when in hot pressing, the temperature is controlled to be 70-85% of the melting point of the matrix metal, and the time is less than or equal to 90 min;
or
Hot-pressing the annealed powder to obtain a finished product; when in hot pressing, the temperature is controlled to be 70-85% of the melting point of the matrix metal, and the time is less than or equal to 90 min;
the other particle powder is selected from at least one of silicon dioxide, granular graphite, flake graphite, hard ceramic, aluminum oxide, silicon carbide, titanium carbide, tungsten carbide and high-entropy alloy;
step five
Sintering the cold pressed compact obtained in the fourth step in a protective atmosphere or a vacuum atmosphere; obtaining a finished product;
the sintering temperature is 60-80% of the melting point of the base metal, and the heat preservation time is more than or equal to 10 min.
2. A method for preparing an ultrafine carbon particle reinforced metal matrix composite according to claim 1; it is characterized in that; under a protective atmosphere; heating the short carbon fiber bundle to 650-800 ℃, and carrying out heat preservation treatment for 20-90 min; obtaining degummed short carbon fiber; the diameter of the short carbon fiber bundle is 6-8 mu m, and the length of the short carbon fiber bundle is 1-4 mm.
3. A method for preparing an ultrafine carbon particle reinforced metal matrix composite according to claim 1; it is characterized in that; in the first step, the volume ratio of the degummed short carbon fiber to the matrix metal powder is 2-19: 1-3; in the first step, the mass percentage of the short carbon fiber in the degummed short carbon fiber and the matrix metal powder is 20-90%.
4. A method for preparing an ultrafine carbon particle reinforced metal matrix composite according to claim 1; it is characterized in that; under a protective atmosphere; in the first step, according to the mass ratio, grinding balls: (the degummed short carbon fiber + matrix metal powder) is 1: 5-8.
5. A method for preparing an ultrafine carbon particle reinforced metal matrix composite according to claim 1; it is characterized in that; the matrix metal is at least one selected from copper, iron, nickel, chromium, manganese and silver.
6. A method for preparing an ultrafine carbon particle reinforced metal matrix composite according to claim 1; it is characterized in that; the particle size of the matrix metal powder is 30-250 mu m; the particle size of the other particle phase powder is 10-400 mu m.
7. A method for preparing an ultrafine carbon particle reinforced metal matrix composite according to claim 1; it is characterized in that; in the first step, the rotating speed of the high-energy ball milling is 220-350 r/min, and the ball milling time is 6-14 h.
8. A method for preparing an ultrafine carbon particle reinforced metal matrix composite according to claim 1; it is characterized in that; in the fourth step, the powder after the reduction annealing and other particle powder are put into a V-shaped mixer to be stirred uniformly; the stirring speed of the V-shaped mixer is 80-120r/min, and the mixing time is 2-5 h.
9. A method for preparing an ultrafine carbon particle reinforced metal matrix composite according to claim 1; it is characterized in that; in the fourth step of the method, the first step of the method,
the pressure of the cold press molding is 200-600 MPa, and the pressure maintaining time is 20-30 s;
the pressure of the hot pressing is 200-600 MPa; the hot pressing temperature is 70% -85% of the melting point of the matrix metal, and the heat preservation and pressure maintaining time is 2-90 min.
10. A method for preparing an ultrafine carbon particle reinforced metal matrix composite according to claim 1; it is characterized in that;
in the obtained finished product, the particle size of the carbon particles is 1-3 mu m;
in the obtained finished product, the mass percentage of the carbon particles is less than or equal to 20 percent.
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