CN110257738A - A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites - Google Patents
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites 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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- 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 present invention relates to the preparation methods of ultra-fine carbon particle enhancing metal-base composites, belong to technical field of composite preparation.Preparation method are as follows: first pass through and short carbon fiber is subjected to degumming process, the short carbon fiber of degumming process and metal powder are obtained into the metal powder for the ultra-fine carbon particle insertion that surface carbon is removed by ball-milling technology appropriate and carbon elimination-reducing process again, again as raw material, obtaining ultra-fine carbon particle by traditional mixing-compacting-sintering process enhances metal-base composites.Ultra-fine carbon particle structure proximate of the invention is in carbon fiber, granularity tiny (1~3 μm) and narrow particle size distribution, uniformly it is embedded in inside metal powder, of the invention designed and preparation ultra-fine carbon particle enhancing metal-base composites has both the high-strength and high ductility of metal, the performances such as corrosion-resistant, and the performances such as the thermal conductivity of carbon fiber, wearability, anti-oxidant, preparation process is simple, at low cost.
Description
Technical field
The present invention relates to the preparation methods of ultra-fine carbon particle enhancing metal-base composites, belong to composite material technology of preparing
Field.
Background technique
Carbon Fibre Reinforced Metal Matrix Composites show excellent mechanical property, wearability, heat-resisting quantity, resistance to electric arc and burn
The series of advantages such as corrosion and good self-lubrication have now been widely used in machinery as a kind of metal-base composites
The fields such as manufacture, aerospace.In particular for properties of carbon fiber reinforced copper composite therein, be widely used in manufacture brush,
Bearing shell, sliding block, electric shock, cooling integrated plate, pantograph pan etc..But because there is a large amount of active official in carbon fiber surface
It can roll into a ball, therefore with other metal mixing process, easily reunite, it is difficult to disperse, it is caused to be unevenly distributed in the base.
For this problem, researcher is proposed with dispersing agent disperse carbon fibers, carbon fiber surface metal lining, Yi Jiyong
Carbon fiber powder substitutes the methods of carbon fiber.But metal lining technical matters long flow path, process cycle are complicated, equipment investment is big, work
Skill is complicated, metal lining and is easy to appear evil mind and the even phenomenon of uneven coating.Chinese patent CN103201026A discloses one kind
A kind of carbon microfiber dispersion liquid is provided, make that there is high aggregation force and forms the fine carbon fiber of aggregation organic molten
It is uniformly dispersed in agent, defibering, and forms stable dispersity.It is a kind of to be dispersed with the micro- of fine carbon fiber in organic solvent
Fine carbon dispersion liquid uses macromolecule dispersing agent, and the size of the aggregation of fine carbon fiber contained in the dispersion liquid
It is 5 μm or less.Chinese patent CN 108103422A discloses a kind of plating Cu short carbon fiber reinforced Cu based composites, passes through powder
The property such as the density, hardness and conductivity that last metallurgy is prepared for short carbon fiber reinforced Cu based composites to improve Cu based composites
Energy.Use 380 DEG C of calcination 30min for preferable carbon fiber except adhesive process；Compared with ultrasonic disperse and magnetic agitation, use is electronic
Short carbon fiber good dispersion when stirring, and Electroless Cu Plating coating even compact.It is compound with the increase of plating Cu short carbon fiber content
Downward trend is presented in the density and conductivity of material, and hardness presentation first improves the trend reduced afterwards, wherein in the plating short carbon fiber of Cu
When dimension hplc is up to 12.5%, Cu based composites hardness number highest；Plate the physical property of the short carbon fiber Cu based composites of Cu
Better than the short carbon fiber material for not plating Cu.
Chinese patent CN103333473A discloses the composite material and its processing work of a kind of carbon fiber or carbon fiber powder
Skill, according to mass percent, comprising: (1) using unsaturated polyester resin or epoxy resin as matrix: 35%~55%；(2)
Carbon fiber or boron fibre: 2%~20%；(3) micro- glass marble or carbonization silicon ball: 5%~15%；(4) carbon fiber powder 35%~
55%；(5) copper powder or copper alloy powder: 2%~20%.The composite material of carbon fiber provided by the invention or carbon fiber powder,
With very high specific strength, specific modulus, the structural member density which forms is small, and grinding effect surface is careful, impact resistance,
And resistance coefficient is low, electric conductivity is good.Chinese patent CN105088421B discloses a kind of preparation method of carbon fiber powder, main
Solve the problems, such as that energy consumption high efficiency existing in the prior art is low, the system of carbon fiber powder of the present invention
Preparation Method, comprising the following steps: (1) continuous carbon fibre and the thermoplastic resin under molten condition is clipped, grind, mix
To the mixture of carbon fiber-containing powder and the thermoplastic resin；(2) above-mentioned mixed with the good solvent dissolution of above-mentioned thermoplastic resin
Close the thermoplastic resin in object；(3) it is separated by solid-liquid separation and obtains the technical solution of the carbon fiber powder, preferably solve the technology
Problem can be used in the industrial production of carbon fiber powder.Chinese patent CN 104098081B discloses a kind of small draw ratio carbon fiber
Tie up the preparation process of powder, comprising the following steps: A, prick beam；B, it bonds；C, slice or milling；D, it dissolves；E, it separates；F, it purifies.
The present invention provides a kind of preparation process of small draw ratio carbon fiber powder, creates a kind of completely new production technology, is able to produce out
Draw ratio and the smaller carbon fiber powder of fineness, and then the using effect of carbon fiber powder can be greatly improved, promote industry and enterprise
Development.For the agglomeration traits for solving carbon fiber powder, Chinese patent CN 104088132B discloses a kind of carbon fiber powder surface and changes
Property method, step be first to carbon fiber powder carry out air calcination pretreatment, then by pretreated carbon fiber powder immerse aoxidize
Liquid carries out surface and is modified, and finally starts the cleaning processing to obtain the modified carbon fiber powder in surface to modified carbon fiber powder.
The method of the present invention has obtained modified carbon fiber powder with good solvent wellability and dispersion stabilization, answers with matrix
Interface adhesive strength when conjunction is preferable.
Summary of the invention
The present invention provides a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites, the simple process and low
Tiny carbon particle being uniformly embedded into metal powder for solving similar carbon fiber structural of cost, and be embedded in carbon particle
Metal powder causes to spread not exclusively between metallic particles, be sintered unsound for after raw material, part carbon is exposed to outside metallic particles
Problem, metal powder obtained have both the thermal conductivity, resistance to of the high-strength and high ductility of metal, the performances such as corrosion-resistant and carbon fiber
The performances such as mill property, anti-oxidant, and preparation process is simple, it is at low cost.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention, includes the following steps:
Step 1
By setting ratio, with short carbon fiber and parent metal powder after degumming is taken, high-energy ball milling is then carried out, is mixed
Powder；
The revolving speed of the high-energy ball milling is 220~350r/min, and Ball-milling Time is more than or equal to 6h；
Step 2
Under an oxygen-containing atmosphere, pre-oxidation treatment is carried out to mixed-powder obtained by step 1；Obtain powder to be restored；It is described pre-
The temperature of oxidation processes is 250~400 DEG C, and the processing time is 10-60min, preferably 20-40min；
Step 3
Under reducing atmosphere, reduced anneal processing is carried out to powder to be restored obtained by step 2；At the reduced anneal
The temperature of reason is 0.3~0.65 times of parent metal fusing point, and annealing time is more than or equal to 30min, preferably 30~60min,
Annealing atmosphere is H2, one of CO or the reduction of a variety of reducing atmospheres, obtain only it is internal include carbon particle metal powder；
Step 4
Powder after annealing is uniformly mixed, then cold-press moulding with other particle powders, obtains cold pressing base；
Or
By the powder cold-press moulding after annealing, cold pressing base is obtained；
Or
Powder after annealing is uniformly mixed with other particle powders, then hot forming, obtains finished product；When hot pressing, control
Temperature processed is the 70%~85% of parent metal fusing point, the time is less than or equal to 90min；
Or
By the powder hot-pressing forming after annealing, finished product is obtained；When hot pressing, controlled at the 70% of parent metal fusing point
~85%, the time is less than or equal to 90min；
Step 5
Under protective atmosphere or vacuum atmosphere, first cold pressing base obtained by step 3 is sintered；Obtain finished product；
The sintering temperature is the 60%~80% of parent metal fusing point, and soaking time is more than or equal to 10min, preferably 10
~200min, further preferably 0.5~3h.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；Under protective atmosphere；By short carbon
Fibre bundle is heated to 650~800 DEG C of isothermal holding 20-90min；Obtain short carbon fiber after degumming.Preferably, the short carbon fiber
Tieing up beam diameter is 6~8 μm, 1~4mm of length.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention is under protective atmosphere；Step 1
In, the volume ratio of short carbon fiber and parent metal powder is 2~19:1~3 after matching the degumming taken.Preferably 1~16:1.Make
It is further preferred；In step 1, match after the degumming taken in short carbon fiber and parent metal powder, matter shared by short carbon fiber
Measuring percentage composition is 20~90%.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；Under protective atmosphere；Step 1
In, it counts in mass ratio, abrading-ball: (short carbon fiber+parent metal powder after degumming)=1:5~8.Preferably 1:6~7.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；Parent metal be selected from iron, copper,
At least one of iron, nickel, chromium, manganese, silver.
Preferably, the partial size of described matrix metal powder is 30~250 μm；The partial size of other particle phase powder
It is 10~400 μm.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；In step 1, the high energy ball
The revolving speed of mill is 220~350r/min, and Ball-milling Time is 6~14h.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；It is described oxygenous in step 2
Atmosphere is preferably air.
Industrially in application, the temperature and time of pre-oxidizing stage wants strict control；No person can seriously affect final production
The content of C and the mechanical property of final products in product.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；In step 3, the reproducibility
Atmosphere has H2, at least one of CO constitutes.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；In step 4, by reduced anneal
Powder and other particle powders afterwards, which is put into V-type batch mixer, to be stirred until homogeneous；The mixing speed of V-type batch mixer is 80-120r/
Min, 2~5h of incorporation time.Other described particle powders are selected from silica, granular graphite, flaky graphite, hard pottery
At least one of porcelain, aluminium oxide, silicon carbide, titanium carbide, tungsten carbide, high-entropy alloy；Other described particles account for total mass of raw material
0~45%.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；In step 4,
The pressure of the cold moudling is 200~600MPa, and the dwell time is 20~30s；
The pressure of the hot pressing is 200~600MPa；Hot pressing temperature is the 70%~85% of described matrix melting point metal,
The heat-insulation pressure keeping time is 2-90min, preferably 10-30min.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；In gained finished product, carbon particle
Partial size is 1~3 μm.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；In gained finished product, carbon particle
Mass percentage is less than or equal to 20%, preferably 1~20%.
A kind of preparation method of ultra-fine carbon particle enhancing metal-base composites of the present invention；In gained finished product, ultra-fine carbon
The structure of grain is similar to carbon fiber.
A kind of preparation method of carbon particle enhancing metal-base composites of the present invention；The short carbon fiber is that degumming process is short
Carbon fiber.Existing carbon fiber surface cladding solidification organic colloid layer on the market, it is necessary to by degumming process, to remove carbon fiber
Surface size agent increases the roughness of carbon fiber surface, so that subsequent (grinding) processing can release " the constraint/limit of sizing agent
System ", and the impurity of carbon fiber surface is eliminated, otherwise percentage of damage is very low.In the present invention, the length of strict control raw material short carbon fiber
The product spent and be necessary for after degumming process can its object is to cooperate rotational speed of ball-mill and mill ball and proportion of the invention
To realize the fine of carbon fiber and the insertion in metallic particles well, in conjunction with the annealing after ball milling, can obtain
It is embedded in the metal powder of ultra-fine carbon particle.
In a kind of of the invention designed and preparation carbon particle enhancing metal-base composites, the granularity of ultra-fine carbon particle is only
It is 1~3 μm, and narrow particle size distribution, degree of purity is high, structural integrity and similar carbon fiber, therefore its height for remaining carbon fiber is led
Electrical conductivity, wearability and the excellent characteristics such as anti-oxidant.
The present invention attempts for the first time, and the short carbon fiber prepared using degumming process technique passes through the height of appropriate ball milling parameter
Energy ball milling and annealing process prepare the metal powder for being embedded in ultra-fine carbon particle；Based on this, metal powder is enhanced using carbon particle
End substitution metal powder is raw material, and in conjunction with carbon elimination-deoxidization technique, high performance carbon particle enhancing is can be obtained in repressed-sintering
Metal-base composites.Composite material obtained has both the thermally conductive of the high-strength and high ductility of metal, the performances such as corrosion-resistant and carbon fiber
The performances such as electric conductivity, wearability, anti-oxidant, and preparation process is simple, it is at low cost.A kind of of the invention designed and preparation carbon
The application of grain enhancing metal-base composites, including be used for the fields such as Heat Conduction Material, conductive material, friction material etc..
Principle and advantage:
The selection and degumming process technique of short carbon fiber.For the selection of short carbon fiber, since carbon fiber surface exists greatly
The active function groups of amount, therefore be directly crushed with long carbon fiber, it is easy to reunite between fiber, it can not be crushed, therefore select short carbon
Fiber can avoid this problem.For the processing method of short carbon fiber, using degumming combination ball-milling technology, this is because commercially available
Carbon fiber surface cladding solidification colloid layer, it is necessary to by degumming process, to remove carbon fiber surface sizing agent, so that subsequent (mill
It is broken) " constraint/limitation " that can release sizing agent is handled, and the impurity and activity of carbon fiber surface are eliminated using degumming tech
Functional group, otherwise percentage of damage is very low, and the optimization of rotational speed of ball-mill and mill ball and proportion, can be very good to realize the super of carbon fiber
Refinement obtains the metal or alloy powder that the ultra-fine carbon particle of similar carbon fiber structural is uniformly embedded into, solve carbon fiber with
Metal powder easy self-assemble and the problem of be uniformly distributed in metallic composite in mixing process.
The selection of surface carbon elimination-deoxidization technique.The densified sintering product of powder relies primarily on intergranular atom diffusion and carries out,
The oxidation film of surface of metal particles and heterogeneous phase will become the obstruction interface of sintering, reduce the sintering densification between powder particle.
It is naked outside metal powder although can realize carbon in the base evenly dispersed with carbon particle enhancing metal powder substitution metal powder
The carbon of dew also counteracts that the sintering between metallic particles is spread.It is well known that carbon is under aerobic environment, at a temperature of 250~300 DEG C
It can aoxidize to form CO2, therefore suitable oxidation technology in short-term is selected, it can remove the carbon of metal powder surface, be conducive to subsequent metal
The progress of particle sintering.Low-temperature treatment in short-term under aerobic environment can make simultaneously although the carbon of metal surface can be removed
A degree of oxidation occurs for the parent metals such as copper, nickel, silver, in order to restore this part metals, therefore after carbon elimination technique, carries out
The reduction treatment of metal powder can not only remove the oxidation film of metal powder, can also eliminate metal powder surface impurity and structure
Defect is conducive to the subsequent compacting sintering of powder, and obtains the ultra-fine carbon particle of structural integrity and approximate carbon fiber.
The preparation process is simple, at low cost, by the regulation of degumming-ball-milling treatment and carbon elimination and reducing process parameter,
It realizes using the carbon particle enhancing metal powder of similar carbon fiber structural as the preparation of the metal-base composites of raw material.
The powder morphology that directly commercially available short carbon fiber is directly obtained by high-energy ball milling is as shown in Figure 2.It is de- by 1000 DEG C
The powder morphology that the short carbon fiber of glue processing is obtained by high-energy ball milling is as shown in Figure 3.By the short carbon fiber of 700 DEG C of degumming process
The powder morphology obtained by excessively high (600r/min) or too low (150r/min) revolving speed ball milling is as shown in Figure 4.By 700 DEG C of degummings
The short carbon fiber 250r/min high-energy ball milling method of processing enhances metal powder in conjunction with the carbon particle of 800 DEG C of annealing preparations
Pattern and Raman map and size distribution difference are as shown in Figure 5,6.Directly using carbon particle enhancing metal powder as raw material, do not appoint
The composite material of where reason preparation is as shown in Fig. 7.Increased with the carbon particle that surface carbon elimination is handled and does not carry out sequential reduction annealing
Strong metal powder is raw material, and the composite material of preparation is as shown in Figure 8.Carbon particle enhancing metal powder is subjected to the annealing of surface carbon elimination and is gone back
Original annealing, the composite material of preparation are as shown in Figure 9.
By Fig. 2~4 it is found that short carbon fiber is without degumming process or degumming process temperature be excessively high or high-energy ball milling
Revolving speed is too fast or too slow, or handles without subsequent anneal, all cannot achieve the ultra-fine carbon particle of approximate carbon fiber structural
Preparation.By Fig. 5~6 it is found that combining suitable high-energy-milling and subsequent high-temperature annealing process using degumming process, not only
The broken of short carbon fiber is realized, also can get the ultra-fine carbon particle of structural integrity and approximate carbon fiber, to make ultra-fine carbon
Grain gives full play to its advantage.But there is the exposed of a large amount of carbon particles on the surface of carbon particle enhancing metal powder, this will be hindered in subsequent
The progress of sintering.It is without any processing by Fig. 7 and Fig. 8 it is found that directly using carbon particle enhancing metal powder as raw material, or only do
Carbon elimination processing, the carbon particle enhancing metal powder without reduced anneal is raw material, through mixing-compacting-sintering composite material
In due to carbon interface obstruction, lead to that there are a large amount of holes.As shown in Figure 9, it anneals and goes back using the surface carbon elimination of parameter optimization
Former annealing process realizes the densified sintering product between metallic particles, and it is multiple to obtain the Metal Substrate that carbon particle is uniformly distributed, porosity is small
Condensation material, gained composite property is excellent and uniform, has good market prospects.
In short, the present invention have preparation process simple (only degumming, ball milling, carbon elimination annealing in short-term, deoxidized annealing), at
Sheet is cheap, gained carbon particle enhances metal-base composites function admirable and uniform, has good market prospects.
Detailed description of the invention
Attached drawing 1 is the flow chart of one of preparation method that carbon particle provided by the invention enhances metal-base composites；
Attached drawing 2 is the powder SEM pattern for directly directly obtaining commercially available short carbon fiber by high-energy ball milling；
Attached drawing 3 is the powder SEM for obtaining the short carbon fiber of 1000 DEG C of degumming process and electrolytic copper powder by high-energy ball milling
Pattern；
Attached drawing 4 is excessively high (600r/min) or too low to pass through the short carbon fiber of 700 DEG C of degumming process with electrolytic copper powder
The powder SEM pattern that (150r/min) revolving speed ball milling obtains；
Attached drawing 5 is that the short carbon fiber of 700 DEG C of degumming process prepared by the present invention and electrolytic copper powder pass through 250r/min high
Energy ball-milling method, the powder SEM pattern of preparation；
Attached drawing 6 is that the short carbon fiber of 700 DEG C of degumming process prepared by the present invention and electrolytic copper powder pass through 250r/min high
Energy ball-milling method, the Raman map of the powder of preparation；
Attached drawing 7 is directly to pass through 250r/min high-energy ball milling method with the short carbon fiber of 700 DEG C of degumming process and electrolytic copper powder
The carbon particle enhancing copper powder of preparation is raw material, does not do the composite material of any carbon elimination and reduction treatment preparation；
Attached drawing 8 is to prepare the short carbon fiber of 700 DEG C of degumming process by 250r/min high-energy ball milling method with electrolytic copper powder
Carbon particle enhance copper powder, after 280 DEG C of surface carbon eliminations anneal 15min, do not carry out sequential reduction annealing, then pass through mixing-pressure
System-sintering preparation Cu-base composites；
Attached drawing 9 is to prepare the short carbon fiber of 700 DEG C of degumming process by 250r/min high-energy ball milling method with electrolytic copper powder
Carbon particle enhance copper powder, after 280 DEG C of surface carbon eliminations anneal 15min and 350 DEG C of hydrogen reducings annealing 30min, then by mixed
Material-compacting-sintering preparation Cu-base composites.
As can be seen from Figure 1 the preparation flow for the ultra-fine carbon particle that the present invention designs, specifically: firstly, degumming process
Short carbon fiber, high-energy ball milling degumming carbon fiber, the carbon particle enhancing metal powder surface carbon elimination for secondly obtaining high-energy ball milling are pre-
Oxidation processes, then the powder after pre-oxidation is made annealing treatment under reducing atmosphere protection, to restore powder surface oxidation
Film and removal surface defect, impurity, carry out conventional mixing-compacting-sintering processes again later, and obtaining carbon particle enhances Metal Substrate
Composite material.
By Fig. 2 to Fig. 4 it is found that short carbon fiber is excessively high without special carbonization treatment or carbonization treatment temperature, or it is high
Energy rotational speed of ball-mill is too fast or too slow, or handles without subsequent anneal, all cannot achieve the ultra-fine carbon of approximate carbon fiber structural
Particle is embedded in the preparation of the metal composite powder of copper particle.
As shown in Figure 5, degumming process combines suitable high-energy-milling and subsequent high-temperature annealing process, original short carbon
Fibre bundle, which is interrupted, to be in granular form, and is embedded in inside copper particle, and the partial size of carbon particle is about 1~3 μm, and carbon particle enhances metal powder
Surface have the exposed of a large amount of carbon particles.
It will be appreciated from fig. 6 that Raman spectrum analysis is shown, the degree of orientation of grain structure shown in fig. 5 is low, close with carbon fiber structural
Seemingly, fault of construction is slightly increased.
It is without any processing by Fig. 7-Fig. 8 it is found that directly using it as raw material, or carbon elimination processing is only done, without reduction
The carbon particle enhancing metal powder of annealing is raw material, all cannot achieve the sintering densification between metal powder granulates.
As shown in Figure 9, it is realized between metallic particles using the surface carbon elimination annealing of parameter optimization and reduced anneal technique
Densified sintering product obtains the metal-base composites that carbon particle is uniformly distributed, porosity is small.
Specific embodiment
Below with reference to attached drawing of the invention, technical solution of the present invention is clearly and completely described, it is clear that retouched
The embodiment stated is only a part of the embodiment in technical solution recorded in the present invention, instead of all the embodiments.It is based on
The embodiment of the present invention, every other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, protection scope of the present invention is belonged to.
Comparative example 1
Prepared Cu-base composites in this comparative example 1, include following components by percentage to the quality:
Short carbon fiber 5.0%, zirconium carbide 1%, electrolytic copper powder 96%.The partial size of zirconium carbide is 100 μm, the grain of electrolytic copper powder
Diameter is 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Directly using commercially available carbon fiber as object, without any pre- place
Reason, is added in ball-grinding machine with electrolytic copper powder and carries out high-energy ball milling, electrolytic copper powder and short carbon fiber are distinguished by mass percentage
For 80% and 20%, revolving speed 250r/min, Ball-milling Time 6h, the ball of ball milling is stainless steel ball, ratio of grinding media to material 5:1.Short carbon
Fiber is simultaneously unbroken, is sticked at ball milling tank skin, and the pattern of composite powder is as shown in Figure 2 after processing.
Composite powder, the zirconium carbide that directly certain proportion is prepared are mixed in V-type batch mixer, obtain mixed powder.Later
It is cold-pressed at room temperature, pressing pressure 450MPa, dwell time 20s, the Cu-base composites green compact of preparation is in hydrogen
Pressure sintering under atmosphere protection, in 950 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 10~15 DEG C/min, are obtained
To 1 exemplar of comparative example.The tensile strength of the Cu-base composites of preparation is 230MPa.
Comparative example 2
Prepared Cu-base composites in this comparative example 2, include following components by percentage to the quality:
Short carbon fiber 5.0%, zirconium carbide 1%, electrolytic copper powder 96%.The partial size of zirconium carbide is 100 μm, the grain of electrolytic copper powder
Diameter is 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is added through 1000 DEG C of degumming process with electrolytic copper powder
High-energy ball milling is carried out into ball-grinding machine, electrolytic copper powder and short carbon fiber are respectively 80% and 20% by mass percentage, revolving speed
For 250r/min, Ball-milling Time 6h, the ball of ball milling is stainless steel ball, ratio of grinding media to material 5:1.Short carbon fiber and be not apparent from it is broken,
The pattern of composite powder is as shown in Figure 3 after processing.
Composite powder, the zirconium carbide that directly certain proportion is prepared are mixed in V-type batch mixer, obtain mixed powder.Later
It is cold-pressed at room temperature, pressing pressure 450MPa, dwell time 20s, the Cu-base composites green compact of preparation is in hydrogen
Pressure sintering under atmosphere protection, in 950 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 10~15 DEG C/min, pressure
Power is 0.5MPa, obtains 2 exemplar of comparative example.The tensile strength of the Cu-base composites of preparation is 243MPa.
Comparative example 3
Prepared Cu-base composites in this comparative example 3, include following components by percentage to the quality:
Short carbon fiber 5.0%, zirconium carbide 1%, electrolytic copper powder 96%.The partial size of zirconium carbide is 100 μm, the grain of electrolytic copper powder
Diameter is 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is added through 700 DEG C of degumming process with electrolytic copper powder
High-energy ball milling, revolving speed 600r/min, Ball-milling Time 8h are carried out into ball-grinding machine, the ball of ball milling is stainless steel ball, sphere diameter
It is added according to a certain ratio for 3mm~10mm, ratio of grinding media to material 6:1.Short carbon fiber is simultaneously not apparent from broken, most of deposition ball milling tank decks
The pattern of composite powder is as shown in Figure 4 at portion's lid, after processing.
Composite powder, the zirconium carbide that directly certain proportion is prepared are mixed in V-type batch mixer, obtain mixed powder.Later
It is cold-pressed at room temperature, pressing pressure 450MPa, dwell time 20s, the Cu-base composites green compact of preparation is in hydrogen
Pressure sintering under atmosphere protection, in 950 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 10~15 DEG C/min, pressure
Power is 0.6MPa, obtains 3 exemplar of comparative example.The tensile strength of the Cu-base composites of preparation is 252MPa.
Comparative example 4
Prepared Cu-base composites in this comparative example 4, include following components by percentage to the quality:
Short carbon fiber 5.0%, zirconium carbide 1%, electrolytic copper powder 96%.The partial size of zirconium carbide is 100 μm, the grain of electrolytic copper powder
Diameter is 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is through 700 DEG C of degumming process 60min, with electrolytic copper powder
It being added in ball-grinding machine and carries out high-energy ball milling, revolving speed 250r/min, Ball-milling Time 8h, the ball of ball milling are stainless steel ball,
Ratio of grinding media to material is 6:1, obtains ultra-fine carbon particle insertion copper powder, and pattern and Raman map are respectively as shown in Fig. 5~6.
Ultra-fine carbon particle insertion copper powder, the zirconium carbide that directly certain proportion is prepared are mixed in V-type batch mixer, are mixed
Powder.It is cold-pressed at room temperature later, pressing pressure 450MPa, dwell time 20s, the Cu-base composites pressure of preparation
Base pressure sintering under hydrogen atmosphere protection, in 950 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 10~15
DEG C/min, pressure 0.65MPa, 4 exemplar of comparative example is obtained, pattern is as shown in Figure 7.Its porosity is up to 10%, and metal
Non- diffusion-sintering between particle.The tensile strength of the Cu-base composites of preparation is 248MPa.
Comparative example 5
Prepared Cu-base composites in this comparative example 5, include following components by percentage to the quality:
Short carbon fiber 5.0%, zirconium carbide 1%, electrolytic copper powder 96%.The partial size of zirconium carbide is 100 μm, the grain of electrolytic copper powder
Diameter is 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is through 700 DEG C of degumming process 60min, with electrolytic copper powder
It being added in ball-grinding machine and carries out high-energy ball milling, revolving speed 250r/min, Ball-milling Time 8h, the ball of ball milling are stainless steel ball,
Ratio of grinding media to material is 6:1, obtains ultra-fine carbon particle insertion copper powder.By carbon particle enhancing copper powder in 280 DEG C of surface carbon eliminations annealing 15min
Afterwards, sequential reduction annealing is not carried out, obtains the carbon particle insertion copper oxide particle of surface carbon removal.
Ultra-fine carbon particle insertion cupric oxide powder, the zirconium carbide that certain proportion is prepared are mixed in V-type batch mixer, are mixed
Powder.It is cold-pressed at room temperature later, pressing pressure 450MPa, dwell time 20s, the Cu-base composites pressure of preparation
Base pressure sintering under hydrogen atmosphere protection, in 950 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 10~15
DEG C/min, pressure 0.55MPa, 5 exemplar of comparative example is obtained, pattern is as shown in Figure 8.Its porosity is 6%, part metals
Intergranular diffusion sintering is not fine and close.The tensile strength of the Cu-base composites of preparation is 265MPa.
Comparative example 6
Prepared iron base composite material in this comparative example 6, includes following components by percentage to the quality:
Short carbon fiber 5.0%, ferrochrome 10%, reduced iron powder 40%.The partial size of ferrochrome is 100 μm, reduced iron
The partial size of powder is 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is through 700 DEG C of degumming process 60min, and also
Former iron powder, which is added in ball-grinding machine, carries out high-energy ball milling, revolving speed 250r/min, Ball-milling Time 6h, and the ball of ball milling is stainless
Steel ball, ratio of grinding media to material 6:1 obtain ultra-fine carbon particle insertion iron powder.Carbon particle enhancing iron powder is annealed in 350 DEG C of surface carbon eliminations
After 15min, sequential reduction annealing is not carried out, obtains the carbon particle insertion ferric oxide particles of surface carbon removal.
Ultra-fine carbon particle insertion brown iron oxide, the ferrochrome that certain proportion is prepared are mixed in V-type batch mixer, are mixed
Close powder.It is cold-pressed at room temperature later, pressing pressure 450MPa, dwell time 20s, the iron base composite material pressure of preparation
Base pressure sintering under hydrogen atmosphere protection, in 1050 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove are 10~15
DEG C/min, pressure 0.45MPa, obtain 6 exemplar of comparative example.Its porosity is 12%, and diffusion-sintering is not fine and close between metallic particles.
The tensile strength of the iron base composite material of preparation is 380MPa.
Comparative example 7
Prepared iron base composite material in this comparative example 7, includes following components by percentage to the quality:
Short carbon fiber 5.0%, ferrochrome 10%, reduced iron powder 40%.The partial size of ferrochrome is 100 μm, reduced iron
The partial size of powder is 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is through 700 DEG C of degumming process 60min, and also
Former iron powder, which is added in ball-grinding machine, carries out high-energy ball milling, revolving speed 250r/min, Ball-milling Time 6h, and the ball of ball milling is stainless
Steel ball, ratio of grinding media to material 6:1 obtain ultra-fine carbon particle insertion iron powder.Carbon particle enhancing iron powder is annealed in 850 DEG C of surface carbon eliminations
After 50min, then in 350 DEG C of hydrogen reducings annealing 20min, obtained carbon particle insertion ferric oxide particles are due to oxidizing temperature
Excessively high, the time is too long, causes to be difficult to be reduced.
Ultra-fine carbon particle insertion iron powder, the ferrochrome that certain proportion is prepared are mixed in V-type batch mixer, are mixed
Powder.It is cold-pressed at room temperature later, pressing pressure 450MPa, dwell time 20s, the iron base composite material green compact of preparation
The pressure sintering under hydrogen atmosphere protection, in 1050 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove be 10~15 DEG C/
Min, pressure 0.8MPa obtain 7 exemplar of comparative example.Its porosity is 18%, since iron oxidation is serious between metallic particles, diffusion
It is sintered not fine and close.The tensile strength of the iron base composite material of preparation is only 187MPa.
Comparative example 8
Prepared nickel-base composite material in this comparative example 8, includes following components by percentage to the quality:
Short carbon fiber 10%, aluminium oxide 5%, electrolytic nickel powder 85%.The partial size of aluminium oxide is 50 μm, and carbon particle is embedded in copper powder
Partial size be 120 μm, the partial size of electrolytic nickel powder is 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is through 720
DEG C degumming process 60min, is added in ball-grinding machine with electrolytic nickel powder and carries out high-energy ball milling, revolving speed is 250r/min, is obtained
Ultra-fine carbon particle is embedded in nickel powder.By carbon particle enhancing nickel powder after 350 DEG C of surface carbon eliminations anneal 30min, sequential reduction is not carried out
Annealing obtains the carbon particle insertion nickel oxide particle of surface carbon removal.
Carbon particle insertion nickel oxide powder, the aluminium oxide prepared according to the above ratio are mixed in V-type batch mixer, obtain mixed powder.
It is cold-pressed at room temperature later, pressing pressure 450MPa, dwell time 20s, the nickel-base composite material green compact of preparation exists
Pressure sintering under hydrogen atmosphere protection, in 1000 DEG C of sintering 2h, pressure is 0.8 MPa, the heating rate and rate of temperature fall of stove
It is 10~15 DEG C/min, obtains 8 exemplar of comparative example.Its porosity is 15%, and diffusion-sintering is not fine and close between part metals particle.
The tensile strength of the nickel-base composite material of preparation is 550MPa.
Embodiment 1
Prepared Cu-base composites in embodiment 1, include following components by percentage to the quality:
Short carbon fiber 5.0%, zirconium carbide 1%, electrolytic copper powder 96%.The partial size of zirconium carbide is 100 μm, the grain of electrolytic copper powder
Diameter is 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is through 700 DEG C of degumming process 60min, with electrolytic copper powder
It being added in ball-grinding machine and carries out high-energy ball milling, revolving speed 250r/min, Ball-milling Time 8h, the ball of ball milling are stainless steel ball,
Ratio of grinding media to material is 6:1, obtains ultra-fine carbon particle insertion copper powder.By carbon particle enhancing copper powder in 280 DEG C of surface carbon eliminations annealing 15min
Afterwards, then in 350 DEG C of hydrogen reducings annealing 30min, the carbon particle insertion copper particle of surface carbon removal is obtained.
Ultra-fine carbon particle insertion copper powder, the zirconium carbide that certain proportion is prepared are mixed in V-type batch mixer, obtain mixed powder
Material.It is cold-pressed at room temperature later, pressing pressure 450MPa, dwell time 20s, the Cu-base composites green compact of preparation
The pressure sintering under hydrogen atmosphere protection, in 950 DEG C of sintering 2h, the heating rate and rate of temperature fall of stove be 10~15 DEG C/
Min, pressure 0.9MPa, obtain 1 exemplar of embodiment, and pattern is as shown in Figure 9.Its porosity is 3%, is spread between metallic particles
Densified sintering product.The tensile strength of the Cu-base composites of preparation is 450MPa.
Embodiment 2
Prepared iron base composite material in embodiment 2, includes following components by percentage to the quality:
Short carbon fiber 10%, ferrochrome 10%, reduced iron powder 80%.The partial size of ferrochrome is 100 μm, reduced iron powder
Partial size be 120 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is through 750 DEG C of degumming process 30min, with reduction
Iron powder, which is added in ball-grinding machine, carries out high-energy ball milling, revolving speed 250r/min, Ball-milling Time 8h, and the ball of ball milling is stainless steel
Ball, ratio of grinding media to material 6:1 obtain ultra-fine carbon particle insertion iron powder.By carbon particle enhancing iron powder in 350 DEG C of progress pre-oxidation treatments
15min；Then in 350 DEG C of hydrogen reducings annealing 20min, the carbon particle insertion iron powder of surface carbon removal is obtained.
Ultra-fine carbon particle insertion iron powder, the ferrochrome that certain proportion is prepared are mixed in V-type batch mixer, obtain mixed powder
Material.It is cold-pressed at room temperature later, pressing pressure 450MPa, dwell time 20s, the iron base composite material green compact of preparation
The pressure sintering under vacuum protection, in 1050 DEG C of sintering 2h, pressure is 0.8 MPa, and the heating rate and rate of temperature fall of stove are equal
For 10~15 DEG C/min, 2 exemplar of embodiment is obtained.Its porosity is 2.5%, and diffusion-sintering is fine and close between metallic particles.Preparation
The tensile strength of iron base composite material is 746MPa.
Embodiment 3
Prepared nickel-base composite material in embodiment 3, includes following components by percentage to the quality:
Short carbon fiber 10%, aluminium oxide 5%, electrolytic nickel powder 85%.The partial size of aluminium oxide is 40 μm, the partial size of electrolytic nickel powder
It is 150 μm.The diameter of short carbon fiber is 6 μm, length 2mm.Short carbon fiber is through 700 DEG C of degumming process 60min, with also electrolytic nickel powder
It being added in ball-grinding machine and carries out high-energy ball milling, revolving speed 250r/min, Ball-milling Time 6h, the ball of ball milling are stainless steel ball,
Ratio of grinding media to material is 6:1, obtains ultra-fine carbon particle insertion iron powder.By carbon particle enhancing nickel powder in 300 DEG C of progress pre-oxidation treatments
10min；Then in 250 DEG C of hydrogen reducings annealing 30min, the carbon particle insertion nickel powder of surface carbon removal is obtained.
Ultra-fine carbon particle insertion nickel powder, the aluminium oxide that certain proportion is prepared are mixed in V-type batch mixer, obtain mixed powder
Material.It is cold-pressed at room temperature later, pressing pressure 500MPa, dwell time 20s, the nickel-base composite material green compact of preparation
The pressure sintering under hydrogen atmosphere protection, in 1000 DEG C of sintering 2h, pressure 0.8MPa, the heating rate and cooling speed of stove
Rate is 10~15 DEG C/min, pressure 0.8MPa, obtains 3 exemplar of embodiment.Its porosity is 2%, is spread between metallic particles
Densified sintering product.The tensile strength of the nickel-base composite material of preparation is 1220MPa.
Claims (10)
1. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites, it is characterised in that；Include the following steps:
Step 1
By setting ratio, with short carbon fiber and parent metal powder after degumming is taken, high-energy ball milling is then carried out, mixed powder is obtained
End；
The revolving speed of the high-energy ball milling is 220~350r/min, and Ball-milling Time is more than or equal to 6h；
Step 2
Under an oxygen-containing atmosphere, pre-oxidation treatment is carried out to mixed-powder obtained by step 1；Obtain powder to be restored；The pre-oxidation
The temperature of processing is 250~400 DEG C, and the processing time is 10~60min, preferably 20-40min；
Step 3
Under reducing atmosphere, reduced anneal processing is carried out to powder to be restored obtained by step 2；The reduced anneal processing
Temperature is 0.3~0.65 times of parent metal fusing point, and annealing time is more than or equal to 30min, preferably 30~60min, annealing
Atmosphere is H2, one of CO or the reduction of a variety of reducing atmospheres, obtain only it is internal include carbon particle metal powder；
Step 4
Powder after annealing is uniformly mixed, then cold-press moulding with other particle powders, obtains cold pressing base；
Or
By the powder cold-press moulding after annealing, cold pressing base is obtained；
Or
Powder after annealing is uniformly mixed with other particle powders, then hot forming, obtains finished product；When hot pressing, control temperature
Degree is the 70%~85% of parent metal fusing point, the time is less than or equal to 90min；
Or
By the powder hot-pressing forming after annealing, finished product is obtained；When hot pressing, controlled at parent metal fusing point 70%~
85%, the time is less than or equal to 90min；
Step 5
Under protective atmosphere or vacuum atmosphere, first cold pressing base obtained by step 3 is sintered；Obtain finished product；
The sintering temperature be parent metal fusing point 60%~80%, soaking time be more than or equal to 10min, preferably 10~
200min, further preferably 0.5~3h.
2. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites according to claim 1；Its feature exists
In；Under protective atmosphere；Short carbon fiber beam is heated to 650~800 DEG C of 20~90min of isothermal holding；Obtain short carbon after degumming
Fiber.Preferably, the short carbon fiber beam diameter is 6~8 μm, 1~4mm of length.
3. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites according to claim 1；Its feature exists
In；In step 1, the volume ratio of short carbon fiber and parent metal powder is 2~19:1~3 after matching the degumming taken.Preferably 1
~16:1.As a further preference；In step 1, match after the degumming taken in short carbon fiber and parent metal powder, short carbon
Mass percentage shared by fiber is 20~90%.
4. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites according to claim 1；Its feature exists
In；Under protective atmosphere；It in step 1, counts in mass ratio, abrading-ball: (short carbon fiber+parent metal powder after degumming)=1:5~
8.Preferably 1:6~7.
5. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites according to claim 1；Its feature exists
In；Parent metal is selected from least one of copper, iron, nickel, chromium, manganese, silver.
6. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites according to claim 1；Its feature exists
In；The partial size of described matrix metal powder is 30~250 μm；The partial size of other particle phase powder is 10~400 μm.
7. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites according to claim 1；Its feature exists
In；In step 1, the revolving speed of the high-energy ball milling is 220~350r/min, and Ball-milling Time is 6~14h.
8. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites according to claim 1；Its feature exists
In；In step 4, the powder after reduced anneal is put into V-type batch mixer with other particle powders and is stirred until homogeneous；V-type mixing
The mixing speed of machine is 80-120r/min, 2~5h of incorporation time.Other described particle powders are selected from silica, graininess stone
At least one of ink, flaky graphite, hard ceramic, aluminium oxide, silicon carbide, titanium carbide, tungsten carbide, high-entropy alloy；It is described
Other particles account for the 0~45% of total mass of raw material.
9. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites according to claim 1；Its feature exists
In；In step 4,
The pressure of the cold moudling is 200~600MPa, and the dwell time is 20~30s；
The pressure of the hot pressing is 200~600MPa；Hot pressing temperature is the 70%~85% of described matrix melting point metal, and heat preservation is protected
The pressure time is 2~90min, preferably 10-30min.
10. a kind of preparation method of ultra-fine carbon particle enhancing metal-base composites according to claim 1；Its feature exists
In；
In gained finished product, the partial size of carbon particle is 1~3 μm.
In gained finished product, the mass percentage of carbon particle is less than or equal to 20%, preferably 1~20%.
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