CN106363185B - The method for preparing powder metallurgy of nanometer phase/composite metal powder and its block materials - Google Patents
The method for preparing powder metallurgy of nanometer phase/composite metal powder and its block materials Download PDFInfo
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- CN106363185B CN106363185B CN201610737318.7A CN201610737318A CN106363185B CN 106363185 B CN106363185 B CN 106363185B CN 201610737318 A CN201610737318 A CN 201610737318A CN 106363185 B CN106363185 B CN 106363185B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 47
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 23
- 229910052782 aluminium Inorganic materials 0.000 claims description 20
- 239000004411 aluminium Substances 0.000 claims description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- 238000000280 densification Methods 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 239000002905 metal composite material Substances 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
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- 229910052719 titanium Inorganic materials 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
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- 239000011159 matrix material Substances 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 3
- 239000002041 carbon nanotube Substances 0.000 description 24
- 229910021393 carbon nanotube Inorganic materials 0.000 description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 18
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- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 7
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- 229910010271 silicon carbide Inorganic materials 0.000 description 6
- 229910000838 Al alloy Inorganic materials 0.000 description 5
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- 244000291564 Allium cepa Species 0.000 description 1
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- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Powder Metallurgy (AREA)
Abstract
The present invention discloses the method for preparing powder metallurgy of a kind of nanometer of phase/composite metal powder and its block materials, the low speed ball milling of nano-phase powder end, metal powder elder generation through a long time is made metal powder tailpiece by the method, and nanometer is made mutually to be dispersed in the surface or inside of piece metal powder simultaneously, obtain nanometer phase/Metal Flake composite powder;Again through high speed ball milling in short-term, make a nanometer phase/Metal Flake composite powder soldering, obtains a nanometer phase/metallic particles shape composite powder;Evenly dispersed and interface cohesion problem of the nanometer mutually in metallic matrix need to can be solved in the present invention only by adjusting ball milling speed, compare traditional average rate ball milling, nanometer is mutually dispersed more evenly and interface bond strength is higher, and the material property of preparation is more excellent;Process of the present invention is simple, efficient simultaneously, is suitable for batch and prepares.
Description
Technical field
The present invention relates to metal-base composites preparation technical field, specifically a kind of nanometer of phase/composite metal powder and
The method for preparing powder metallurgy of its block materials.
Background technique
In recent years, excellent mechanical of the nanometer phase strengthened metal base composite material due to having both conventional metals based composites
Can and preferable plasticity and toughness, thermal stability and the advantages that machinability, get the attention in recent years, be considered aviation,
The numerous areas such as space flight, traffic, electronics and sports goods have huge application potential.However, various nanometers mutually have it is excellent
Mechanical property, functional characteristic and unique geometric shape, while bringing excellent properties to enhance to metal-base composites,
Also to composite-making process, more stringent requirements are proposed.Studies have shown that the reinforcing effect for giving full play to nanometer phase requires it in base
Meet the requirements simultaneously in body: nanometer is mutually scattered, structural integrity, is combined with matrix, and the metallurgy in the composite material of preparation lacks
It is few etc. to fall into (such as hole, micro-crack, field trash).
Molecular level mixing (Molecular Level Mix), fabricated in situ (In Situ Synthesis), slurry are total
The methods of mixed flakelike powder metallurgical (Flake Powder Metallurgy), can preferably meet and play nanometer phase reinforcing effect
Requirement, but these method processes are relative complex, are difficult to carry out industrialized production;The nanometer prepared using tradition machinery ball-milling method
In phase/metallic composite, the dispersibility and these more above-mentioned methods of structural intergrity of nanometer phase are poor, thus in composite material
There are obvious disadvantages for energy aspect, but are suitable for following large-scale production, have certain industrial applications potentiality.Therefore, how
The evenly dispersed technology of new nanometer phase is developed in mechanical attrition method, and its structural integrity is kept to be combined with matrix, and is made
It is the critical issue in current nanometer phase/metallic composite production and application technology without metallurgical imperfection in standby composite material.
By to the prior art literature search discovery, at present to the problem research mainly by mechanical milling process when
Between, revolving speed carry out unitary variant optimal control.Choi et al. (" The effect of milling conditions on
microstructures and mechanical properties of Al/MWCNT composites”Composites
Part A 43 (2012) 1061-1072) in 425~600rpm high speed ball milling, ball milling are carried out to aluminium and carbon nanotube mixed-powder
Time is more than 10h, and mixed-powder constantly broken, soldering under the impact of steel ball, ultimately forms carbon nanotube/aluminium in mechanical milling process
Form of spherical particles composite powder, but carbon nanotube dispersion effect is bad, and its nanostructure strengthens effect by serious destruction
Fruit is bad.Liu et al. people (" Mechanical alloying of multi-walled carbon nanotubes and
aluminium powders for the preparation of carbon/metal composites”Carbon 47
(2009) 3427-3433) using the mixed-powder of lower rotational speed of ball-mill (300rpm) ball milling aluminium and carbon nanotube, aluminium powder is in steel
The shear action bottom sheet of ball, and carbon nanotube is gradually scattered in the surface of flake aluminum under the rubbing action of steel ball, knot
Structure extent of the destruction is lighter;But carbon nanotube is distributed in flake aluminum surface, in conjunction with not strong;Meanwhile flakelike powder deformability lacks
It loses, aoxidize seriously, there are more metallurgical imperfections in the block materials of preparation, have very high requirement to subsequent machining technology, usually
Large plastometric set technique is needed to promote interface cohesion, eliminate metallurgical imperfection, thus the sample size, the shape that prepare are limited, together
When it is also very high to equipment requirement.Therefore, essentially consist in the shortcomings that the prior art: above-mentioned single average rate ball milling can not meet simultaneously to be received
Rice mutually dispersibility, structural intergrity, in conjunction with matrix, the technical requirements that metallurgical imperfection is few, thus can not be in metal-based compound material
The performance enhancement potentiality of nanometer phase are given full play in material.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of nanometer of phase/composite metal powder and its block
The method for preparing powder metallurgy of body material, the change that sheet metal, nanometer are mutually gradually dispersed under this method combination low speed ball milling condition
The soldering of composite powder, granulation mechanism of Evolution, realize that nanometer is mutually evenly dispersed and good in a metal under shape mechanism and high speed ball milling
It is good to combine, give full play to reinforcing effect of the nanometer mutually in metallic matrix.
To achieve the above object, the technical solution adopted by the present invention is that:
According to the first aspect of the invention, a kind of nanometer of phase/composite metal powder preparation method is provided, comprising:
The low speed ball milling of nano-phase powder end, metal powder elder generation through a long time is made into metal powder tailpiece, and makes nanometer simultaneously
It is mutually dispersed in the surface or inside of piece metal powder, obtains nanometer phase/Metal Flake composite powder;
Again through high speed ball milling in short-term, make a nanometer phase/Metal Flake composite powder soldering, obtains a nanometer phase/metallic particles shape
Composite powder;
The revolving speed of the low speed ball milling is not higher than 300 revs/min, and the high speed rotational speed of ball-mill is not less than corresponding low
1.5 times of fast rotational speed of ball-mill;
The long period low speed ball milling refers to that Ball-milling Time is greater than 6 hours, when the ball milling of high speed in short-term refers to ball milling
Between be not more than 2.5 hours.
Preferably, the low speed rotational speed of ball-mill is 100~200 revs/min.
Preferably, the high speed rotational speed of ball-mill is 250~400 revs/min.
Preferably, the nanometer mutually includes the reinforcement that various characteristic dimensions are nano-scale, including nano-oxide, is received
Rice ceramics, nanocrystalline intermetallics, nano-sized carbon (carbon nanotube, graphene, Nano diamond, nano-sized carbon onion).
Preferably, the metal powder includes aluminium, magnesium, titanium, copper, iron, nickel and its alloy powder.
Preferably, the mass fraction of the nanometer phase is the 0.05~10% of composite powder, it is furthermore preferred that the nanometer phase
Mass fraction be composite powder 0.5~8%, still more preferably, be 0.5~2%.
Preferably, the ratio at the nano-phase powder end and metal powder gross mass and abrading-ball, i.e. material ball ratio are 1:5~1:
50, it is furthermore preferred that the material ball ratio is 1:20.
According to the second aspect of the invention, a kind of nanometer of phase/metal composite block materials powder metallurgy preparation side is provided
Method, the method by the densification of PM technique, obtain nanometer phase/metallic particles shape composite powder obtained above
Nanometer phase/metal composite block materials.
Described PM technique, including compacting, sintering and plastic deformation etc., the mode of the compacting include cold pressing, temperature
Pressure, hot pressing, isostatic cool pressing and hot isostatic pressing etc., the sintering processing include pressureless sintering, hot pressing and hot isostatic pressing etc., and deformation adds
Work mode includes jumping-up, secondary multiple pressure, forging, extruding, rolling etc..
In the present invention, the internal characteristics for distinguishing low speed ball milling and high speed ball milling are that powder caused by ball milling speed changes becomes
The variation of shape mechanism: abrading-ball, which can be analyzed to positive pressure and tangential shearing force, pressure to the active force of powder, mainly to be caused
Powder is plastically deformed, and shearing force mainly causes the dispersion of nanometer phase.In general, rotational speed of ball-mill is low lower than 300 revs/min
Fast ball milling pressure and shearing force are all lower, and the energy of input is lower, and the sheets of powder time is long, and abrading-ball is with the shearing force ratio to powder
Example is higher, thus nanometer can be made mutually gradually to disperse during metal powder tailpiece, and do not cause obviously to nanometer phase structure
It destroys.But as mentioned in the background, nanometer is mutually scattered in powder table in the sheet composite powder of low speed ball milling preparation
Face, in conjunction with weaker, flakelike powder apparent volume is small, deformability is poor, oxidation is serious, is difficult densification.
High speed ball milling stamping press and shearing force are all higher, and the energy of input is high, and nanometer mutually also has little time the work in shearing force
With it is lower realize it is fully dispersed, metal powder rapid piece and by higher stamping press soldering slabbing composite powder soldering in
Granular, not fully dispersed nanometer mutually also by it is buried wherein, while under the effect of higher power, nanometer is mutually being embedded in metal
It is very easy to destroy by serious structure before intragranular.But in high speed mechanical milling process, the multiple soldering of powder forms densification
Graininess composite powder, due to cold welding impact force much higher than conventional powder metallurgical densify pressure, particle interior metal and increase
Strong body is well combined and the defects of hole, micro-crack is seldom, and is conducive to the subsequent densification of graininess composite powder;Meanwhile
Since graininess composite powder size is larger, specific surface area is small, moreover it is possible to oxygen when reducing the exposure of ball milling metal powder in air
Change, avoids introducing additional oxide and be mingled with.In other words, high speed ball milling is unfavorable for the lossless, evenly dispersed of nanometer phase, but advantageous
In nanometer phase/combination of composite metal powder and the reduction of metallurgical imperfection.
Technical solution proposed by the present invention is pressing composite powder first with relatively long time low speed ball action
Gradually piece under power effect, while nanometer is mutually gradually scattered in flakelike powder surface in shearing force, then makes a nanometer phase/gold
Belong to uniform compound flakelike powder cold welding under high speed ball milling to be granulated, under the higher pressure of high speed ball milling, flakelike powder is rapid
Soldering, and shorter Ball-milling Time destroyed caused by nanometer phase structure it is also smaller.Abrading-ball movement velocity is fast, the moment punching of collision
Pressure is very high, the flaky metal powder soldering under pressure that low speed ball milling can be made to obtain, and is locally generating densification
Effect.Graininess composite powder apparent volume is small, carries out the powder such as green compact, densification, deformation processing for graininess composite powder
The microdefect that last metallurgical technology needs to make up during preparing block composite material greatly reduces, and effectively increases a nanometer phase
The metallurgical quality of combination and composite material with metal.
Compared with prior art, the invention has the following advantages:
Compared to the nanometer phase strengthened metal base composite material of average rate ball milling preparation, speed change ball-milling technology institute proposed by the present invention
Composite material obtained had not only had the advantages that low speed ball milling prepared that composite material nanometer is mutually scattered, structural intergrity is good, but also tool
Have the advantages that clipping the ball mill prepare composite material reinforcement body/basal body interface be combined, metallurgical imperfection it is few, be conducive to give full play to and receive
Rice phase reinforcing effect excellent in metallic matrix.
By the control of the parameters such as time, revolving speed in tradition machinery ball-milling technology, speed change ball milling is realized with can be convenient,
Suitable for the compound of various metals, alloy substrate and nano-phase material.
The present invention is simple, efficient, can prepare bulk composite material, is suitable for large-scale production.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
The preparation method of nanometer phase/composite metal powder of the present invention, comprising the following steps:
(1) ball grinder is added after weighing by design proportion in nano-phase powder end and metal powder;
(2) mixed-powder obtains evenly dispersed sheet composite powder through long period low speed ball milling;
(3) sheet composite powder obtains nanometer phase/metallic particles shape composite powder through high speed ball milling in short-term;
On the basis of above-mentioned nanometer phase/metallic particles shape composite powder, pass through the powder such as compacting, sintering and plastic deformation
Metallurgical technology means realize the densification of nanometer phase/metallic particles shape composite powder, obtain nanometer phase/metal composite block material
Material.
Embodiment 1
Carbon nanotube/aluminium composite material
It is greater than 99.5% using purity, the ball aluminum powder that average grain diameter is 10 microns is as metallic matrix powder, using outer
Diameter is 20~40 nanometers, and a length of 2~5 microns of multi-walled carbon nanotube is as nano-phase powder end.
Carbon nanotube/aluminium mixed-powder is placed in planetary ball mill, carbon nanotube mass score is 2%, and ratio of grinding media to material is
It is compound to prepare carbon nanotube/alumina particles shape with 270rpm high speed revolving speed ball milling 1h with 135rpm revolving speed low speed ball milling 8h by 20:1
Powder.
Carbon nanotube/alumina particles shape composite powder is hot-forming at vacuum environment, 300MPa and 550 DEG C, sintering 2h
Afterwards, it is squeezed at 420 DEG C with 1mm/min rate, 25:1 extrusion ratio as pole sample.
Embodiment 2
Graphene/copper composite material
The spherical copper powder prepared using atomization, purity are greater than 99.5%, and average grain diameter is 30 microns;Using redox
The graphene nanometer sheet of method preparation, piece thickness are 1~3 nanometer, and diameter is 0.5~2 micron.
Graphene/copper mixed-powder is placed in stirring ball mill, graphene mass fraction is 0.5%, and quality is added
The stearic acid of score 1%, ratio of grinding media to material 15:1 are placed in planetary ball mill with taking out after 150rpm revolving speed low speed ball milling 6h, with
426rpm high speed revolving speed ball milling 0.5h, prepares graphene/copper graininess composite powder.
By graphene/copper graininess composite powder after cold moudling under 500MPa, under an argon atmosphere, at 950 DEG C
After being sintered 4h, jumping-up to lower upsetting amount is 25% at 700 DEG C, obtains graphene/copper composite material.
Embodiment 3
Nano aluminium oxide/iron composite material
The spherical iron powder prepared using atomization, purity are greater than 98%, and average grain diameter is 45 microns;Average grain diameter is 20nm
γ-Al2O3Particle.
By Al2O3/ iron composite powder end is placed in stirring ball mill, Al2O3Mass fraction is 8%, ratio of grinding media to material 25:1,
It to be taken out after 200rpm revolving speed low speed ball milling 10h, is placed in planetary ball mill, with 426rpm high speed revolving speed ball milling 1.5h, preparation
Nano aluminium oxide/iron particle shape composite powder.
Nano aluminium oxide/iron particle shape composite powder is formed in a vacuum, at 1000 DEG C with 500MPa pressure hot pressing 2h
Afterwards, it is 50% that lower amount is rolling at 900 DEG C, is squeezed at 420 DEG C with 1mm/min rate, 25:1 extrusion ratio as pole sample
Product.
Embodiment 4
Nano boron carbide/magnesium base composite material
It is greater than 99.5% using purity, the ball-shaped magnesite powder that average grain diameter is 35 microns;The nanometer that average grain diameter is 50 nanometers
Boron carbide particles.
Nano boron carbide/magnesium composite powder is placed in stirring ball mill, nano boron carbide mass fraction is 5%, ball
Material is than being that 15:1 is placed in planetary ball mill with taking out after 200rpm revolving speed low speed ball milling 6h, with 400rpm high speed revolving speed ball milling
1h prepares nano boron carbide/magnesium granules shape composite powder.
By nano boron carbide/magnesium granules shape composite powder after cold moudling under 500MPa, after being sintered 2h at 600 DEG C,
It is squeezed at 350 DEG C with 1mm/min rate, 25:1 extrusion ratio as pole sample.
Embodiment 5
Nano titanium carbide/titanium composite material
It is greater than 99.5% using purity, the sized spherical titanium powder that average grain diameter is 45 microns;The nanometer that average diameter is 50 nanometers
Titanium carbide granule.
Nano titanium carbide/titanium composite powder is placed in planetary ball mill, nano boron carbide mass fraction is 3%, ball
Material is than being that 25:1 is placed in planetary ball mill with taking out after 200rpm revolving speed low speed ball milling 8h, with 400rpm high speed revolving speed ball milling
2h prepares nano titanium carbide/titanium graininess composite powder.
Nano aluminium oxide/iron particle shape composite powder is formed in a vacuum, at 1100 DEG C with 500MPa pressure hot pressing 2h
Afterwards, it is 50% that lower amount is rolling at 600 DEG C, obtains nano titanium carbide/titanium composite material.
Embodiment 6
Nanometer silicon carbide/Al alloy composite
Use average grain diameter for 35 microns of spherical Al alloy powder (- 4% magnesium of aluminium);The nanometer that average grain diameter is 80 nanometers
Silicon-carbide particle.
Nanometer silicon carbide/aluminium alloy compound powder is placed in planetary ball mill, nanometer silicon carbide mass fraction is
5%, ratio of grinding media to material 20:1 are placed in planetary ball mill with taking out after 135rpm revolving speed low speed ball milling 8h, are turned with 270rpm high speed
Fast ball milling 1h prepares nanometer silicon carbide/aluminum alloy granule shape composite powder.
By nanometer silicon carbide/aluminum alloy granule shape composite powder after cold moudling under 500MPa, 4h is sintered at 570 DEG C
Afterwards, sample is square with 2mm/min rate, the extruding of 10:1 extrusion ratio at 370 DEG C.
Comparing embodiment 1
Carbon nanotube/aluminium composite material
Carbon nanotube/aluminium composite material for compareing with embodiment 1 is greater than 99.5% using purity, and average grain diameter is
10 microns of ball aluminum powder uses outer diameter for 20~40 nanometers as metallic matrix powder, and a length of 2~5 microns of multi wall carbon is received
Mitron is as nano-phase powder end.
Carbon nanotube/aluminium mixed-powder is placed in planetary ball mill, carbon nanotube mass score is 2%, and ratio of grinding media to material is
20:1 prepares carbon nanotube/aluminium composite powder with 135rpm revolving speed low speed ball milling 9h.
Carbon nanotube/alumina particles shape composite powder is hot-forming at vacuum environment, 300MPa and 550 DEG C, sintering 2h
Afterwards, it is squeezed at 420 DEG C with 1mm/min rate, 25:1 extrusion ratio as pole sample.
Comparing embodiment 2
Carbon nanotube/aluminium composite material
Carbon nanotube/aluminium composite material for compareing with embodiment 1 is greater than 99.5% using purity, and average grain diameter is
10 microns of ball aluminum powder uses outer diameter for 20~40 nanometers as metallic matrix powder, and a length of 2~5 microns of multi wall carbon is received
Mitron is as nano-phase powder end.
Carbon nanotube/aluminium mixed-powder is placed in planetary ball mill, carbon nanotube mass score is 2%, and ratio of grinding media to material is
20:1 prepares carbon nanotube/aluminium composite powder with 270rpm revolving speed low speed ball milling 9h.
Carbon nanotube/alumina particles shape composite powder is hot-forming at vacuum environment, 300MPa and 550 DEG C, sintering 2h
Afterwards, it is squeezed at 420 DEG C with 1mm/min rate, 25:1 extrusion ratio as pole sample.
Comparing embodiment 3
Graphene/copper composite material
Graphene/copper composite material for compareing with embodiment 2, the spherical copper powder prepared using atomization, purity are big
In 99.5%, average grain diameter is 30 microns;The graphene nanometer sheet prepared using oxidation-reduction method, piece thickness are 1~3 nanometer, directly
Diameter is 0.5~2 micron.
Graphene/copper mixed-powder is placed in stirring ball mill, graphene mass fraction is 0.5%, and quality is added
It is compound to prepare graphene/copper with taking-up after 150rpm revolving speed low speed ball milling 6.5h by the stearic acid of score 1%, ratio of grinding media to material 15:1
Powder.
By graphene/copper graininess composite powder after cold moudling under 500MPa, under an argon atmosphere, at 950 DEG C
After being sintered 4h, jumping-up to lower upsetting amount is 25% at 700 DEG C, obtains graphene/copper composite material.
Technological parameter in 1. embodiment of table
The mechanical property of 2. embodiment of table
The method for preparing powder metallurgy of nanometer phase/composite metal powder and its block materials of the present invention, the block of acquisition
Composite material, wherein nanometer be mutually uniformly dispersed, structure it is intact, be well combined with matrix, the metallurgical imperfection in material is few, is mentioned
The embodiment of confession the result shows that, the phase of nanometer prepared by the method for the invention/metallic composite has that mould tough balance good
The characteristics of.
The method of the present invention is not necessarily to extras compared to prior powder metallurgy method, it is only necessary to which simply adjusting ball milling parameter is
Can, it is applied widely, facilitate preparation bulk composite material.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (6)
1. a kind of nanometer of phase/composite metal powder preparation method, characterized by comprising:
The low speed ball milling of nano-phase powder end, metal powder elder generation through a long time is made into metal powder tailpiece, and keeps nanometer mutually equal simultaneously
The even surface or inside for being scattered in piece metal powder obtains nanometer phase/Metal Flake composite powder;
Again through high speed ball milling in short-term, make a nanometer phase/Metal Flake composite powder soldering, it is compound to obtain a nanometer phase/metallic particles shape
Powder;
The prolonged low speed ball milling refers to: low speed rotational speed of ball-mill is 100~200 revs/min, and it is small that Ball-milling Time is greater than 6
When;
The ball milling of high speed in short-term refers to: high speed rotational speed of ball-mill is 250~400 revs/min, and Ball-milling Time is small no more than 2.5
When;
In the high speed ball milling and the low speed ball milling: the ratio at the nano-phase powder end and metal powder gross mass and abrading-ball,
I.e. material ball ratio is 1:5~1:50;
The nanometer mutually includes the reinforcement that various characteristic dimensions are nano-scale, and the nanometer is mutually nano-oxide, nanometer
At least one of ceramics, nanocrystalline intermetallics, nano-sized carbon.
2. according to claim 1 nanometer of phase/composite metal powder preparation method, characterized in that the metal powder
For at least one of aluminium, magnesium, titanium, copper, iron, nickel and its alloy powder.
3. according to claim 1 nanometer of phase/composite metal powder preparation method, characterized in that the nanometer phase
Mass fraction is nanometer phase/composite metal powder 0.05~10%.
4. according to claim 1-3 nanometer of phase/composite metal powder preparation method, characterized in that described
Material ball ratio be 1:20.
5. a kind of nanometer of phase/metal composite block materials method for preparing powder metallurgy, it is characterised in that: the method will be above-mentioned
Nanometer phase/metallic particles shape composite powder that any one of claim 1-4 is obtained is obtained by the densification of PM technique
Nanometer phase/metal composite block materials.
6. according to claim 5 nanometer of phase/metal composite block materials method for preparing powder metallurgy, feature exist
In: the PM technique, including compacting, sintering and plastic deformation.
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