CN106312057A - Powder metallurgy preparation method for nano-particle reinforced ultra-fine grain metal-matrix composite - Google Patents
Powder metallurgy preparation method for nano-particle reinforced ultra-fine grain metal-matrix composite Download PDFInfo
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0057—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on B4C
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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Abstract
The invention provides a powder metallurgy preparation method for a nano-particle reinforced ultra-fine grain metal-matrix composite. According to the method, a metal-matrix grain refining process and a nano-particle dispersing process are carried out in steps. The method comprises the steps that firstly, micro-nano flaky metal-matrix powder is prepared in advance; nano-particles and the flaky metal-matrix powder are stirred and mixed in a stirrer at the high speed under protective atmosphere, and by means of high shear force and pressure generated between stirring blades and a tank body, the nano-particles are uniformly dispersed to the surface of the micro-nano flaky metal-matrix powder; through short-time mechanical ball-milling treatment, the nano metal particles are embedded into the micro-nano flaky metal-matrix powder, so that composite powder of nano-particle reinforced metal is obtained; and compression moulding, sintering and compacting treatment are conducted, so that the ultra-fine grain metal-matrix composite with the nano-particles uniformly dispersed is obtained. By means of the powder metallurgy preparation method, time and energy are saved; cost is low; the application range is wide; and the prepared material is high in comprehensive mechanical performance and has large-scale application potential.
Description
Technical field
The present invention relates to metal-base composites technical field, in particular it relates to a kind of nano-particle reinforcement Ultra-fine Grained gold
The method for preparing powder metallurgy of metal-matrix composite material.
Background technology
The metal-base composites being composited by metallic matrix and reinforcement has the ductility of metal and reinforcement concurrently
The characteristic such as high rigidity, high-modulus, has important purposes and irreplaceability in the high-tech area such as transportation, Aero-Space.
Along with the further development of science and technology, the high-tech area such as transportation, the Aero-Space combination property to metal-base composites
It is also proposed higher requirement, the nanorize of reinforcement granule and the nanocrystalline strengthening of the Ultra-fine Grained of metallic matrix is a new generation's gold
The developing direction of metal-matrix composite material, therefore, the technology of preparing of exploitation nano-particle reinforcement ultra-fine crystal composite material is domestic and international
The focus of research.
Find according to technical literature retrieval, the major technique hands of current nano-particle reinforcement ultrafine grain metal based composites
Section can be divided into two big classes.The first kind is liquid phase process, is first distributed in melt by nano-particle, the block then obtained solidification
Body material imposes large plastometric set so that crystal grain refines, and nano-particle distribution is more uniform；Equations of The Second Kind is in powder metallurgy
Mechanical alloying method, will carry out long-time high-energy ball milling by globular metallic powder after nanometer reinforcement granule mechanical mixture, logical
Cross the repetition cold welding of powder body, shattering process so that the nano-particle of cluster is gradually distributed in matrix, simultaneously the crystalline substance of parent metal
Grain is refined as Ultra-fine Grained.Bulk composite is prepared finally by densification process such as sintering, extruding.Liquid method is owing to receiving
Rice grain easily in process of setting segregation to grain boundaries, and the existence of nano-particle to matrix deformation have the biggest obstruction, hold
Easily make to deform uneven, higher to deformation processing equipment requirements.And mechanical alloying method has, and designability is strong, the scope of application
Wide advantage, becomes the main method of preparation bulk nano-particle reinforcement ultra-fine crystal composite material.Although Mechanical Alloying
Can preferably realize the dispersion of nano-particle, but there is also following weak point: original metal powder is usually tens microns
Spherical powder, big with nanometer reinforcement size difference, the mechanical milling process taken long enough is to realize crystal grain refinement and dispersion, consumption
Time laborious, and be easily caused topical nanoparticulate and again reunite；Such as document (Hesabi Z R, Materials Science and
Engineering:A, 2006,428 (1): 159-168.) by diameter 50 μm aluminium powder and the Al of 5vol.% diameter 35nm2O3Granule
It is blended directly in planetary ball mill with 250 revs/min of ball millings 24 hours, finds initial stage (in the 8h) nanoparticle agglomerates at ball milling
On alumina particles surface, the ball milling requiring more than 20 hours just can make nanometer Al2O3Granule preferably embeds inside aluminum substrate, reaches
To steady statue.While it is true, still have many nanoparticle agglomerates together, cause strengthening effect poor.Existing machinery closes
The shortcoming of aurification technology is: the ball milling starting stage, and nano-particle is wrapped in matrix powder with the form of cluster, and this is accomplished by
Nano-particle could be further distributed into by the ball milling i.e. large deformation process repeatedly of parent metal powder for a long time again
In matrix.Total Ball-milling Time is long, and energy consumption is high.
Summary of the invention
For defect of the prior art, it is an object of the invention to provide a kind of nano-particle reinforcement ultrafine grain metal base multiple
The method for preparing powder metallurgy of condensation material, has metallic matrix crystal grain by the composite prepared by the method thin, and nanometer increases
The strong finely dispersed feature of body, and there is good intensity and plasticity and toughness coupling, the more conventional powder metallurgy of comprehensive mechanical property shows
Write and improve.
For realizing object above, the present invention by the following technical solutions:
The method for preparing powder metallurgy of a kind of nano-particle reinforcement ultrafine grain metal based composites, by metallic matrix crystal grain
Thinning process is carried out with the dispersive process substep of nano-particle, described method: the most previously prepared micro-nano sheet metal substrate
Powder；Again by nano-particle and micro-nano sheet metal substrate powder under protective atmosphere, through high-speed stirring in short-term in agitator
Mix mixing, utilize the high shear force and pressure produced between stirring vane and tank body, make nano-particle evenly spread to micro-nano
The surface of shape metallic matrix powder；Processed by mechanical ball milling in short-term further, nano-particle is embedded micro-nano sheet metal
In matrix powder, it is thus achieved that the composite particles of nanoparticle-reinforced metal；Finally by compressing, sintering and densification,
Obtain nano-particle homodisperse ultrafine grain metal based composites.
Concrete, said method comprising the steps of:
Said method comprising the steps of:
(1) spherical metallic matrix powder is carried out ball milling, obtain the micro-nano sheet metal base with bigger serface
Body powder, and make the crystallite dimension of metallic matrix be reduced to Ultra-fine Grained scope simultaneously；
(2) micro-nano sheet metal substrate powder step (1) obtained is added to according to design proportioning with nano-particle
In agitator, high-speed stirred mixing is utilized to make nano-particle evenly spread to micro-nano sheet metal substrate powder under protective atmosphere
The surface at end, it is thus achieved that the homodisperse mixed-powder of nano-particle；
(3) mixed-powder obtaining step (2) carries out mechanical ball milling process in short-term so that nano-particle is embedded into micro-nano
In rice sheet metal substrate powder, it is thus achieved that the finely dispersed composite powder of nano-particle；
(4) composite powder by obtaining step (3) is pressed into base, sintering and densification, it is thus achieved that nanometer
Granule strengthens ultrafine grain metal based composites.
Preferably, in (1), the diameter of described spherical metallic matrix powder is between 1～100 μm；
Preferably, in (1), the micro-nano sheet metal substrate powder grain size obtained after ball milling is 50～500nm
Between, specific surface area is 10～30 times of original spherical metallic matrix powder, thickness between 0.1～2 μm, sheet footpath is 5
～500 between μm.
Preferably, described mechanical milling process is wet grinding or dry grinding, and the one in water, ethanol or kerosene selected by wet grinding solvent.
It is highly preferred that described wet grinding or dry milled process need adition process controlling agent, the process control agent choosing of dry grinding
With the one in methanol, ethanol or stearic acid or combination, the process control agent of wet grinding is selected in titanate esters, oleic acid or imidazoline
One or combination.
Preferably, in (1), described spherical metallic matrix powder is aluminum, copper, magnesium, titanium, ferrum, nickel and alloy powder thereof
In one or more.
Preferably, in (2), described agitator is to have one to be provided with the puddler of four stirring vanes, the closeest
The tank body of envelope, wherein: the slit size between described stirring vane and described tank body is 1～5mm；After the unlatching of described agitator at a high speed
The described stirring vane rotated produces an annular space for mixed-powder in described tank body；The rotating speed model of described puddler
Enclose is 0～10000 rev/min.
Preferably, in (2), described high-speed stirred mixing, is in the stirring that setting speed is 1500～10000 revs/min
Device is carried out；The time of high-speed stirred mixing is 3～20 minutes；After having mixed, the shape of micro-nano sheet metal substrate powder
Looks are basically unchanged, and nano-particle is dispersed in micro-nano sheet metal substrate powder surface.
Preferably, in (2), described nano-particle is carborundum, titanium carbide, boron carbide, boron nitride, aluminium oxide, oxidation
One or more in silicon, titanium oxide, zirconium oxide, copper oxide, diamond.
Preferably, in (2), described protective atmosphere selects the one in nitrogen, argon or helium, is used for preventing at a high speed
In stirring mixing and Mechanical Milling Process, micro-nano sheet metal substrate powder aoxidizes.
Preferably, in (3), described mechanical ball milling in short-term processes, and refers to: under protective atmosphere, and the ball-milling treatment time is
30～90 minutes, and without any process control agent, under the high-speed impact of ball-milling medium ball, micro-nano in mechanical milling process
The weldering of shape metallic matrix powder surface is combined together, thus nano-particle is embedded into the internal shape of micro-nano sheet metal substrate powder
Become composite powder.
Preferably, in (3), in described composite powder: the characteristic size of nano-particle between 5～300nm, nanometer
The total content of grain is 0.1～20wt.%.
It is highly preferred that described nano-particle total content is 0.5～10wt.%.
Preferably, in (4), described sintering process is atmosphere sintering or vacuum heating-press sintering, discharge ion bundle sintering, heat
Isostatic sintering, sintering temperature is higher than the decomposition temperature of the process control agent added in mechanical milling process but is less than the molten of metallic matrix
Point.
Preferably, in (4), described densification includes: cold pressing, isostatic cool pressing, temperature and pressure, pressureless sintering, hot pressing burn
One or more in knot, high temperature insostatic pressing (HIP), and follow-up extruding, forging, jumping-up, rolling mill practice.
The dispersive process substep of metallic matrix grain refinement process with nano-particle is carried out by the present invention, solves nanometer
Grain Quick uniform dispersion in metallic matrix:
First, replacing the spherical powder of tradition tens microns for mixing raw material with micro-nano flaky metal powder, it compares table
Area is 10～30 times of globular metallic powder, and bigger serface is conducive to dispersed on its surface of nano-particle, and
Being simultaneously achieved the crystal grain refinement of matrix during preparing micro-nano flaky metal powder, crystallite dimension is 50～500nm
Between；
Secondly, the most high-revolving stirring mixing method in agitator under protective atmosphere used, utilize stirring vane
High speed rotating (1500～10000 revs/min) from the slit (1～5mm) between tank body produced by powerful shearing force and different
Mutual extruding force between powder makes nanocluster be opened, and makes nano-particle be evenly affixed to micro-nano sheet metal substrate
Powder surface, thus (3～10 minutes) realize nano-particle at micro-nano sheet metal substrate powder table within the extremely short time
The dispersion in face, and the structural deterioration to nanometer reinforcement is little, and degree of scatter is along with spherical metallic matrix Specific Surface Area Measurement
Increase and increase.This is different from traditional mechanical alloying, the crystal grain refinement of matrix alloy in traditional mechanical alloying
The dispersive process of process and nano-particle is Tong Bu carried out, and the change procedure that metal dust experiences in mechanical milling process is lamellar
The large deformation process repeatedly of change-fragmentation-seam-fragmentation again-seam again, nano-particle and matrix powder be simply mixed after by
In the easy agglomeration of nano-particle itself and be available for the reasons such as scattered surface area is less, cause nanoparticle agglomerates at metal powder
Surface, end, along with the nano-particle that carries out of ball milling incorporates in matrix powder with the form of cluster, needs by long ball milling
The i.e. large deformation process repeatedly of parent metal powder improves the dispersibility of nano-particle, the dispersibility of nano-particle and ball milling
Time, rotating speed are directly proportional (time is the longest, rotating speed is the highest, and dispersibility is the best), and preparation method the most provided by the present invention is effective
Shorten the nano-particle homodisperse time；
Finally, use (30～90 minutes) mechanical ball milling in short-term to process and nano-particle is embedded micro-nano sheet metal substrate
In powder, promote the interface cohesion of nano-particle and micro-nano sheet metal substrate powder, then by through follow-up densification
Change process, can obtain nano-particle finely dispersed ultrafine grain metal based composites.
In the present invention, the size of nanometer reinforcement granule is between 5～300nm, and the crystallite dimension of metallic matrix only has hundreds of
Nanometer, the dispersed work hardening capacity that improve Ultra-fine Grained matrix of nano-particle, thus strong giving full play to Ultra-fine Grained
Good plasticity is kept in the case of change and reinforced by nanoparticles double mechanism.
In the present invention, described Ultra-fine Grained refers to that final crystallite dimension is between 100～1000nm.
Nano-particle reinforcement ultrafine grain metal based composites of the present invention, as the matter of the nano-particle of reinforcement
Amount mark can need arbitrarily to regulate and control in the range of 0.1～20wt.% according to design.Metal-based compound material prepared by the present invention
The room temperature strength of material is more than 8% more than 300MPa, elongation percentage.
Compared with prior art, the present invention has a following beneficial effect:
(1) only needing very short time can realize nano-particle to mix with the uniform of metallic matrix, dispersing uniformity is high；
(2) whole preparation process by short time ball milling prepare micro-nano flaky metal powder, in short-term high-speed stirred mixing, short
Time machinery ball-milling treatment three part composition, the dispersive process of the grain refinement process of metallic matrix with nano-particle is separated, whole
Individual process with tradition high-energy ball milling mixed process compared with, energy-and time-economizing, reduce cost；
(3) metal-base composites of final Nano-size Reinforced Particle homodisperse Ultra-fine Grained matrix, is possible not only to play
Complex intensifying and Ultra-fine Grained strengthen dual strengthening mechanism, and nano-particle improves ultra-fine at dispersed within Ultra-fine Grained
The work hardening capacity of brilliant matrix, thus while obtaining high strength and modulus, keep good plasticity；
(4) preparation method is applied widely, can prepare bulk composite, be suitable for large-scale production.
Accompanying drawing explanation
By the detailed description non-limiting example made with reference to the following drawings of reading, the further feature of the present invention,
Purpose and advantage will become more apparent upon:
Fig. 1 is the method flow schematic diagram of one embodiment of the invention；
Fig. 2 is that in one embodiment of the invention, sheet thickness is the SEM photograph of the flake aluminum of 1～2 μm；Wherein: (a) is flaky aluminum
Powder diametric(al) photo, (b) is flake aluminum thickness direction photo；
Fig. 3 is the SEM photograph of the nano silicon carbide granulate of a size of 50nm in one embodiment of the invention；
Fig. 4 is through high-speed stirred mixed SiC/Al mixed-powder in one embodiment of the invention, wherein: (a) is mixed
Closing powder photo, (b) is mixed-powder partial enlargement photo；
Fig. 5 is the composite particles that in one embodiment of the invention, composite powder is formed after short time mechanical ball milling.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following example will assist in the technology of this area
Personnel are further appreciated by the present invention, but limit the present invention the most in any form.It should be pointed out that, the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement.These broadly fall into the present invention
Protection domain.
Metal dust used in following example is reaction-injection moulding, and purity is all higher than 99%, and remaining chemical reagent is equal
For analytical pure.All embodiments are all carried out according to the technological process shown in Fig. 1, the room-temperature mechanical property of material in all embodiments
All carrying out with reference to " GB/T228.1-2010 ", rate of extension is 0.5mm/min.
Embodiment 1: nanometer silicon carbide/aluminum (SiC/Al) composite
As it is shown in figure 1, the method for preparing powder metallurgy of a kind of nano-particle reinforcement ultrafine grain metal based composites, described
Method is as follows in order to the process preparing nanometer silicon carbide/aluminum (SiC/Al) composite:
Take 1000g 10 μm fine aluminium (Al) powder to be placed in stirring ball mill, using dehydrated alcohol as solvent, add 40g
Titanate esters is as mechanical milling process controlling agent, and ratio of grinding media to material is 20:1, after with the rotating speed ball milling 1h of 352 revs/min, filtering, being vacuum dried
Obtain flake aluminum, the sheet footpath of flake aluminum be 20～40 μm, sheet thickness be 1～2 μm, radius-thickness ratio be 20～40；
Taking 100g nanometer silicon carbide (SiC) granule, particle size average-size is 50nm, adds in dehydrated alcohol and surpasses
Sound cleans, filters, is dried；
Above-mentioned flake aluminum 950g, nano silicon carbide granulate 50g (volume fraction of SiC is 4.2%) are added agitator
In, it is passed through nitrogen as protective atmosphere, takes out after operating 5 minutes with rotating speed 1750 revs/min；Mixed-powder is joined planet ball
In grinding machine, with 6mm stainless steel ball as ball-milling medium, ratio of grinding media to material 10:1, take out after 60 minutes compound with 426 revs/min of ball millings of rotating speed
Powder, and the base substrate of a diameter of 80mm of cold moudling under the pressure of 200MPa；Then by base substrate at 580 DEG C of vacuum heating-press sinterings
3 hours, squeeze with the extrusion ratio of 25:1, the extruding rate of 2mm/min after being then incubated 1 hour in the vacuum press stove of 440 DEG C
Pressure is the pole of a diameter of 10mm.
As in figure 2 it is shown, for the SEM photograph of flake aluminum that sheet thickness is 1～2 μm, figure (a) can be seen that flake aluminum surface
Structural integrity, a diameter of 10～50 μm, figure (b) can be seen that flake aluminum thickness is uniform, and thickness is 1～2 μm.
As it is shown on figure 3, be the SEM photograph of the nano silicon carbide granulate of a size of 50nm, owing to particle size is little, nano-sized carbon
Silicon carbide particle is reunited together.
As shown in Figure 4, for through high speed and precision mixed SiC/Al mixed-powder SEM photograph, from Fig. 4, (b) is permissible
What after finding out mixing, nano silicon carbide granulate was highly uniform is dispersed in lamellar aluminum flake surface, and flake aluminum maintains original
Sheet shape (as shown in (a) in Fig. 4).
As it is shown in figure 5, be the composite particles of the 200-400 μm level that high-energy ball milling was formed after 60 minutes, amplify from Fig. 5 b
Particle surface it can be seen that substantially there is no nano silicon carbide granulate on surface, it is seen that by ball milling in short-term really by nano-sized carbon
Silicon carbide particle has been embedded into inside aluminum substrate；The room-temperature mechanical property of the composite finally prepared is shown in Table 1.
Comparative example 1:
Take ball aluminum powder in the same manner as in Example 1 and nano carborundum powder 950g and 50g respectively, be placed directly within planetary
In ball mill, add 2wt.% stearic acid, under argon shield, after being total to ball milling 6 hours with the rotating speeds of 426 revs/min, prepare compound
Powder.This powder is carried out pressed compact, sintering and deformation after unloading and heat treatment according to technique in the same manner as in Example 1, its room temperature
Mechanical property is shown in Table 1.
Embodiment 2: nano boron carbide/magnesium base composite material
As it is shown in figure 1, the method for preparing powder metallurgy of a kind of nano-particle reinforcement ultrafine grain metal based composites, described
Method is as follows in order to the process preparing nano boron carbide/magnesium base composite material:
Take 200g, the ball-shaped magnesite powder end of 30 μm is placed in stirring ball mill, using argon as protective atmosphere, adds 6g hard
Fat acid is as mechanical milling process controlling agent, and ratio of grinding media to material is 20:1, with the rotating speed ball milling 3h of 423 revs/min, it is thus achieved that flake aluminum, lamellar
The sheet footpath of aluminium powder be 50～70 μm, average sheet thickness be 200nm, radius-thickness ratio is more than 200；
Nano boron carbide (B is prepared according to the method in embodiment 14C) powder, nano boron carbide particle mean size is
40nm；
By above-mentioned lamellar magnesium powder 186g, nano silicon carbide boron powder 14g (boron carbide body fraction is 7.5vol.%), add
High-speed stirring mixer, rotating speed 1850 revs/min, operating 7 minutes after take out；Mixed-powder is joined in planetary ball mill, with
6mm stainless steel ball is ball-milling medium, ratio of grinding media to material 10:1, to take out composite powder after 426 revs/min of ball millings of rotating speed 90 minutes, and
Under the pressure of 200MPa, 150 DEG C of base substrates being pressed into a diameter of 40mm；Then by base substrate 580 DEG C of hot pressed sinterings 3 hours, so
After in the vacuum press stove of 350 DEG C, be incubated after 1 hour extrusion ratio, the extruding rate of 2mm/min with 25:1 extrude as diameter
Pole for 8mm；The room-temperature mechanical property of the composite finally prepared is shown in Table 1.
Embodiment 3 nano titanium carbides/titanium composite material
As it is shown in figure 1, the method for preparing powder metallurgy of a kind of nano-particle reinforcement ultrafine grain metal based composites, described
Method is as follows in order to the process preparing nano titanium carbide/titanium composite material:
Taking 500g mean diameter is that 45 μm titanium valves are respectively placed in two planetary ball mill tanks, using argon as protective atmosphere,
Each 2.5g stearic acid that adds is as mechanical milling process controlling agent, and ratio of grinding media to material is 20:1, with the rotating speed ball milling 2h of 426 revs/min, it is thus achieved that sheet
Shape titanium valve, the sheet footpath of lamellar titanium valve be 50～70 μm, average sheet thickness be 300nm, radius-thickness ratio is more than 150；
Above-mentioned lamellar titanium valve 485g, average diameter 10nm nano titanium carbide granule 15g are added in agitator, is passed through argon
As protective atmosphere, take out after operating 10 minutes with rotating speed 2500 revs/min；The mixed-powder of gained is joined planetary ball mill
In, with 10mm stainless steel ball as ball-milling medium, ratio of grinding media to material 20:1, take out composite powder with 500 revs/min of ball millings of rotating speed after 30 minutes
End, and make the base substrate of a diameter of 40mm with hot pressed sintering 3h under the pressure of 500MPa at 1100 DEG C；Roll at 600 DEG C again
System, roll lower amount is 5% point of 10 passes every time, and always rolling lower amount is 50%, the room temperature power of the composite finally prepared
Performance is shown in Table 1.
Embodiment 4: nano-titanium oxide/Al alloy composite
As it is shown in figure 1, the method for preparing powder metallurgy of a kind of nano-particle reinforcement ultrafine grain metal based composites, described
Method is as follows in order to the process preparing nano-titanium oxide/Al alloy composite:
Take 500g, spherical 6061 aluminum (6061Al) alloy powder of 30 μm is placed in stirring ball mill, using argon as
Protective atmosphere, addition 5g stearic acid is as mechanical milling process controlling agent, and ratio of grinding media to material is 20:1, with the rotating speed ball milling 3h of 423 revs/min,
Obtain flake aluminum, the sheet footpath of flake aluminum be 50～70 μm, average sheet thickness be 200nm, radius-thickness ratio is more than 200.
Being averaged particle diameter is 20nm titanium dioxide powder 25g, adds in agitator, be passed through argon together with 475g flake aluminum
As protective atmosphere, take out after operating 10 minutes with rotating speed 2500 revs/min；The mixed-powder of gained is joined planetary ball mill
In, with 6mm stainless steel ball as ball-milling medium, ratio of grinding media to material 10:1, take out composite powder with 426 revs/min of ball millings of rotating speed after 60 minutes,
And cold pressing under the pressure of 300MPa and to make the base substrate of a diameter of 80mm；Then by base substrate 600 DEG C of hot pressed sinterings 3 hours, so
After in the vacuum press stove of 530 DEG C, be incubated after 1 hour extrusion ratio, the extruding rate of 12mm/min with 25:1 extrude as diameter
Pole for 8mm；Then by pole Quenching Treatment 180 DEG C of timeliness 18h after 530 DEG C of insulation 2h, it is thus achieved that final block
Ultra-fine crystal composite material, its room-temperature mechanical property is shown in Table 1.
Embodiment 5: nano aluminium oxide/carbon/carbon-copper composite material
As it is shown in figure 1, the method for preparing powder metallurgy of a kind of nano-particle reinforcement ultrafine grain metal based composites, described
Method is as follows in order to the process preparing nano aluminium oxide/carbon/carbon-copper composite material:
Take 500g, 30 μm fine copper powder are placed in stirring ball mill, using dehydrated alcohol as solvent, add 2g titanate esters
As ball milling controlling agent, ratio of grinding media to material is 20:1, with the rotating speed ball milling 3h of 352 revs/min, filter, be vacuum dried after obtain sheet of copper
Powder, the sheet footpath of copper powder be 40 ± 3 μm, sheet thickness be 500 ± 20nm.
Being averaged particle diameter is 10nm alumina powder 50g, adds in agitator, be passed through argon together with 450g flake copper
As protective atmosphere, take out after operating 12 minutes with rotating speed 3000 revs/min；The mixed-powder of gained is joined planetary ball mill
In, with 10mm stainless steel ball as ball-milling medium, ratio of grinding media to material 15:1, take out composite powder with 400 revs/min of ball millings of rotating speed after 90 minutes
Under end, and 500MPa after cold moudling, in argon gas atmosphere after 950 DEG C of sintering 4h, repeatedly forge and press at 800 DEG C, obtain block and receive
Rice aluminium oxide/carbon/carbon-copper composite material, its room-temperature mechanical property is shown in Table 1.
Table 1 alloying component and room-temperature mechanical property thereof
From table 1 it follows that embodiment 1 compares with comparative example 1, the tensile strength of composite and modulus have bright
Aobvious lifting, shows that the enhancing efficiency of SiC significantly improves, meanwhile maintains good plasticity, elongation percentage reaches 12%, comprehensively
Mechanical property significantly improves.
The present invention by nano-particle and micro-nano sheet metal substrate powder under protective atmosphere in agitator through shorter
Time high-speed stirred mixes, and utilizes the high shear force produced between puddler and tank body and compression stress to make nano-particle dispersed
Surface to flaky metal powder；By the high-energy ball milling of short time, nano-metal particle is embedded in metallic matrix further,
Obtain the composite particles of nanoparticle-reinforced metal, then obtain nano-particle by compressing, sintering and hot extrusion deformation
Homodisperse ultrafine grain metal based composites.By the composite prepared by the method, there is metallic matrix crystal grain thin,
The finely dispersed feature of nano-particle, the dispersed work hardening capacity to improving Ultra-fine Grained matrix of nano-particle has very well
Effect such that it is able to while giving full play to refined crystalline strengthening and complex intensifying, keep good plasticity, comprehensive mechanical property
More conventional powder metallurgy significantly improves.The method time-saving energy-saving of the present invention, improves Ultra-fine Grained multiple while reducing preparation cost
The comprehensive mechanical property of condensation material, and can be used for preparing massive material, there is huge scale application potential.
Above the specific embodiment of the present invention is described.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformation or amendment within the scope of the claims, this not shadow
Ring the flesh and blood of the present invention.
Claims (12)
1. the method for preparing powder metallurgy of a nano-particle reinforcement ultrafine grain metal based composites, it is characterised in that described
Method comprises the following steps:
(1) spherical metallic matrix powder is carried out ball milling, obtain the micro-nano sheet metal substrate powder with bigger serface
End, and make the crystallite dimension of metallic matrix be reduced to Ultra-fine Grained scope simultaneously；
(2) micro-nano sheet metal substrate powder step (1) obtained is added to stirring with nano-particle according to design proportioning
In device, high-speed stirred mixing is utilized to make nano-particle evenly spread to micro-nano sheet metal substrate powder under protective atmosphere
Surface, it is thus achieved that the homodisperse mixed-powder of nano-particle；
(3) mixed-powder obtaining step (2) carries out mechanical ball milling process in short-term so that nano-particle is embedded into micro-nano
In shape metallic matrix powder, it is thus achieved that the finely dispersed composite powder of nano-particle；
(4) composite powder by obtaining step (3) is pressed into base, sintering and densification, it is thus achieved that nano-particle
Strengthen ultrafine grain metal based composites.
The powder metallurgy preparation side of a kind of nano-particle reinforcement ultrafine grain metal based composites the most according to claim 1
Method, it is characterised in that in step (1): the diameter of described spherical metallic matrix powder is between 1～100 μm；After ball milling
The micro-nano sheet metal substrate powder grain size obtained is between 50～500nm, and specific surface area is original spherical gold
Belonging to 10～30 times of matrix powder, thickness is between 0.1～2 μm, and sheet footpath is between 5～500 μm.
The powder metallurgy preparation side of a kind of nano-particle reinforcement ultrafine grain metal based composites the most according to claim 2
Method, it is characterised in that described mechanical milling process is wet grinding or dry grinding, the one in water, ethanol or kerosene selected by wet grinding solvent.
The powder metallurgy preparation side of a kind of nano-particle reinforcement ultrafine grain metal based composites the most according to claim 3
Method, it is characterised in that need adition process controlling agent in described wet grinding or dry milled process, the process control agent of dry grinding selects first
One in alcohol, ethanol or stearic acid or combination, the process control agent of wet grinding selects in titanate esters, oleic acid or imidazoline
Plant or combination.
5. according to the powder smelting of a kind of nano-particle reinforcement ultrafine grain metal based composites described in any one of claim 1-4
Gold preparation method, it is characterised in that described spherical metallic matrix powder is aluminum, copper, magnesium, titanium, ferrum, nickel and alloy powder thereof
In one or more.
The powder metallurgy preparation side of a kind of nano-particle reinforcement ultrafine grain metal based composites the most according to claim 1
Method, it is characterised in that described high-speed stirred mixing, is to enter in the agitator that setting speed is 1500～10000 revs/min
OK, the time of high-speed stirred mixing is 3～20 minutes；After having mixed, the pattern of micro-nano sheet metal substrate powder is basic
Constant, nano-particle is dispersed in micro-nano sheet metal substrate powder surface.
The powder metallurgy preparation side of a kind of nano-particle reinforcement ultrafine grain metal based composites the most according to claim 6
Method, it is characterised in that described agitator is to have a tank being provided with the puddler of four stirring vanes, high-seal
Body, wherein: the slit size between described stirring vane and described tank body is 1～5mm；High speed rotating after the unlatching of described agitator
Described stirring vane can produce an annular space for mixed-powder in described tank body；The range of speeds of described puddler is
0～10000 rev/min.
The powder metallurgy preparation side of a kind of nano-particle reinforcement ultrafine grain metal based composites the most according to claim 1
Method, it is characterised in that described nano-particle is carborundum, titanium carbide, boron carbide, boron nitride, aluminium oxide, silicon oxide, oxidation
One or more in titanium, zirconium oxide, copper oxide, diamond.
9. according to the powder smelting of a kind of nano-particle reinforcement ultrafine grain metal based composites described in any one of claim 6-8
Gold preparation method, it is characterised in that described protective atmosphere is the one in nitrogen, argon or helium.
Prepared by the powder metallurgy of a kind of nano-particle reinforcement ultrafine grain metal based composites the most according to claim 9
Method, it is characterised in that described sintering process is that atmosphere sintering or vacuum heating-press sintering, discharge ion bundle sintering, heat etc. are quiet
Pressure sintering, sintering temperature is higher than in mechanical milling process the decomposition temperature of the process control agent added but is less than the fusing point of metallic matrix；
Described densification includes: cold pressing, isostatic cool pressing, temperature and pressure, pressureless sintering, hot pressed sintering, high temperature insostatic pressing (HIP), and follow-up
One or more in extruding, forging, jumping-up, rolling mill practice.
Prepared by the powder metallurgy of 11. a kind of nano-particle reinforcement ultrafine grain metal based composites according to claim 1
Method, it is characterised in that described mechanical ball milling in short-term processes, and refers to: under protective atmosphere, and the ball-milling treatment time is 30～90
Minute, and without any process control agent, under the high-speed impact of ball-milling medium ball, micro-nano sheet metal in mechanical milling process
The weldering of matrix powder surface is combined together, thus nano-particle is embedded into micro-nano sheet metal substrate powder and is internally formed compound
Powder.
12. according to the powder metallurgy of a kind of nano-particle reinforcement ultrafine grain metal based composites described in claim 1 or 11
Preparation method, it is characterised in that in described composite powder: the characteristic size of nano-particle between 5～300nm, nanometer
Grain total content is 0.1～20wt.%.
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