CN109108298A - A kind of preparation method of high tough hierarchical structure metal-base composites - Google Patents
A kind of preparation method of high tough hierarchical structure metal-base composites Download PDFInfo
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Abstract
The invention patent belongs to materials processing technology field, and in particular to a kind of preparation method of high tough hierarchical structure metal-base composites, the specific steps are as follows: (1) matrix alloy powder is passed through high-energy ball milling, obtain flaky metal powder;(2) by reinforcement, mechanical stirring and ultrasonic disperse in dispersion liquid are mixed with gained flaky metal powder, obtain composite powder I after filtering, drying;(3) composite powder I obtains composite powder II again with ball-type metal powder low energy ball milling;(4) composite powder II partial remelting, thixotropic forming after cold-press moulding under stress, obtains the metal-base composites mixed-powder briquetting of hierarchically organized configuration.The principle of the invention is succinct, easy to operate, safe and reliable, can industrialized production, while improving work efficiency, saved material, ensure that quality, is safe and reliable, application with higher and promotional value.
Description
Technical field
The invention patent belongs to materials processing technology field, particularly belongs to metal-base composites preparation technical field, relates to
And a kind of preparation method of high tough hierarchical structure metal-base composites.
Background technique
Aluminum matrix composite is answered extensively due to having many advantages, such as good thermal stability, high specific stiffness, high specific strength
For fields such as aerospace, military affairs, automobiles.Most of existing researchs are by single reinforcement or hybrid buildup body in matrix
In be uniformly distributed and obtain uniform configuration metal-base composites, can reduce to a certain extent because reinforcement reunite generate
Cross problem of brittle fracture caused by high stress concentrations.However, because of the composite configuration effect for not fully taking into account material, so that material
Though the intensity of material obtains limited improvement, toughness sharply declines, and becomes and hinders metal-base composites in higher level and more
A kind of main bottleneck of wide scope application.Solve the problems, such as that this most effective means is exactly the composite material for preparing hierarchical structure.Point
Level structure be by the soft phase region of matrix of the hard phase region and poor reinforced phase of rich reinforced phase by certain spatial distribution constitute it is non-
Even group of texture type.Hard phase region can effectively play load transmission and strengthen and hinder dislocation motion, play invigoration effect.And soft phase region
It can promote dislocation motion and passivation crack tip, sluggish crack growth rate, play toughening effect.Thus, hierarchical structure is more
Be conducive to play the collaboration coupling effect between the freedom degree and constituent element of composite design, it can be achieved that the excellent intensity of composite material/it is rigid
Degree and plasticity/toughness matching.Therefore, the research of hierarchical structure composite material is carried out in a deep going way, this answers further Metal Substrate of excavating
The performance potential of condensation material and its broader applications is pushed to have great theoretical and practical significance.
Powder metallurgic method is also to prepare the most common method of hierarchical structure composite material at present.Powder metallurgic method reaction temperature
Low (as being lower than Al alloy solidus temperature), sintering time is long (4h or so), and energy consumption is high, and production efficiency is low.Especially, this method
The part compactness of preparation is poor, is difficult to prepare the part of large scale, complicated shape.Although being burnt by microwave sintering, plasma
The technologies such as knot and subsequent secondary operation (such as rolling, mixing yoghurt, hot extrusion) can improve dense structure's property, but increase
Cost, and it is still helpless for preparation larger size, complicated shape part.And near-net-shape is for unmanageable gold
Metal-matrix composite material part is particularly important.Therefore, it is necessary to develop a kind of method for preparing high-performance hierarchical structure composite material.
Thixotropic forming technology can not only substantially reduce, even be eliminated the defects of shrinkage porosite, stomata, and can also near-net-shape it is big
The thin-walled parts of size, complicated shape.The mixed powder of combining powder metallurgy, compaction process and thixotropic forming technology partial remelting,
Forming technology advantage can develop the new method for preparing hierarchical structure composite material.
Summary of the invention
To solve the above-mentioned problems, the invention patent proposes a kind of system of high tough hierarchical structure metal-base composites
Preparation Method can improve existing metal-base composites intensity and toughness mismatch, the problem of dense structure's property difference.
Technical solution are as follows:
A kind of preparation method of high tough hierarchical structure metal-base composites, the specific steps are as follows:
(1) in liquid nitrogen cooling and under protective atmosphere, matrix alloy powder is passed through into high-energy ball milling, obtains flaky metal powder;
Matrix alloy powder particle can be spherical, ellipsoid or wedge-shaped herein;
(2) by reinforcement, mechanical stirring and ultrasonic disperse in dispersion liquid are mixed with gained flaky metal powder, after filtering, drying
Reinforcement uniform adsorption is obtained in the composite powder I on flaky metal powder surface;
(3) again with pellet base alloy powder low energy ball milling, acquisition composite powder I is uniformly distributed in spherical gained composite powder I
Composite powder II around metal powder;Matrix alloy powder particle is spherical or ellipsoid herein, has reached good fill up
Effect;
(4) gained composite powder II cold-press moulding under stress, obtains mixed-powder briquetting;
(5) gained mixed-powder briquetting heats under semi-solid temperature, obtains the semisolid non-dendritic ingot for being suitble to thixotropic forming;
(6) gained semisolid non-dendritic ingot thixotropic forming under corresponding mold temperature, forming pressure, pressure head rate, obtains
Hierarchical structure composite material.
Further, described matrix alloy powder is the Al alloy powders such as Al-Cu, Al-Mg, Al-Si, Al-Zn system, Mg-Al,
The magnesium alloy powders such as Mg-Zn system, kirsites such as ZA8, ZAl2, ZA22, ZA27 system etc., described matrix alloy powder average grain diameter exist
Between 3 ~ 80 μm.
Further, the reinforcement is one of graphene, carbon nanotube, carbon fiber;Wherein, graphene size: thick
Degree is 1 ~ 30nm, 1 ~ 20um of length;Carbon nanotube sizes: 20 ~ 100nm of diameter, 1 ~ 50um of length;Carbon fiber size are as follows: diameter
For 50 ~ 180nm, 1 ~ 20 μm of length.
Further, the dispersion liquid is one of methanol, acetone, ethyl alcohol, deionized water, polyvinyl alcohol.
Further, in step (1) high-energy ball milling condition be 350 ~ 500rpm of revolving speed, 8 ~ 14h of Ball-milling Time, ratio of grinding media to material 20:
1, process control agent stearic acid 2wt.%, cooling medium is liquid nitrogen, and protective gas is argon gas, can prepare piece under the above conditions
Shape metal powder.
Further, low energy ball milling condition is 80 ~ 150rpm of revolving speed, 4 ~ 7h of Ball-milling Time, ratio of grinding media to material 5:1 in step (3), is protected
Shield atmosphere is argon gas.
Further, the reinforcement and the volume ratio of flaky metal powder are 1:10 ~ 30.
Further, the composite powder I is again 1:2 ~ 6 with the volume ratio of ball-type metal powder.
The utility model has the advantages that the present invention compared with the existing technology, the advantage is that present invention improves existing metal-based compound materials
Expect intensity and toughness mismatch, the problem that dense structure's property is poor, part shape is size-constrained.
The principle of the invention is succinct, easy to operate, safe and reliable, can industrialized production, while improving work efficiency, having saved material
Expect, ensure that quality, is safe and reliable, application with higher and promotional value.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
A kind of preparation method of high tough hierarchical structure metal-base composites as described in Figure 1, the specific steps are as follows:
(1) in liquid nitrogen cooling and under protective atmosphere, matrix alloy powder is passed through into high-energy ball milling, obtains flaky metal powder;
(2) by reinforcement, mechanical stirring and ultrasonic disperse in dispersion liquid are mixed with gained flaky metal powder, after filtering, drying
Reinforcement uniform adsorption is obtained in the composite powder I on flaky metal powder surface;
(3) gained composite powder I obtains composite powder I and is uniformly distributed in ball-type metal again with ball-type metal powder low energy ball milling
Composite powder II around powder;
(4) gained composite powder II cold-press moulding under stress, obtains mixed-powder briquetting;
(5) gained mixed-powder briquetting heats under semi-solid temperature, obtains the semisolid non-dendritic ingot for being suitble to thixotropic forming;
(6) gained semisolid non-dendritic ingot thixotropic forming under corresponding mold temperature, forming pressure, pressure head rate, obtains
Hierarchical structure composite material.
Further, described matrix alloy powder is the Al alloy powders such as Al-Cu, Al-Mg, Al-Si, Al-Zn system, Mg-Al,
The magnesium alloy powders such as Mg-Zn system, kirsites such as ZA8, ZAl2, ZA22, ZA27 system etc., described matrix alloy powder average grain diameter exist
Between 3 ~ 80 μm.
Further, the reinforcement is one of graphene, carbon nanotube, carbon fiber;Wherein, graphene size: thick
Degree is 1 ~ 30nm, 1 ~ 20um of length;Carbon nanotube sizes: 20 ~ 100nm of diameter, 1 ~ 50um of length;Carbon fiber size are as follows: diameter
For 50 ~ 180nm, 1 ~ 20 μm of length.
Further, the dispersion liquid is one of methanol, acetone, ethyl alcohol, deionized water, polyvinyl alcohol.
Further, in step (1) high-energy ball milling condition be 350 ~ 500rpm of revolving speed, 8 ~ 14h of Ball-milling Time, ratio of grinding media to material 20:
1, process control agent stearic acid 2wt.%, cooling medium is liquid nitrogen, and protective gas is argon gas.
Further, low energy ball milling parameter is 80 ~ 150rpm of revolving speed, 4 ~ 7h of Ball-milling Time, ratio of grinding media to material 5:1 in step (3), is protected
Shield atmosphere is argon gas.
Further, the reinforcement and the volume ratio of flaky metal powder are 1:10 ~ 30.
Further, the composite powder I is again 1:2 ~ 6 with the volume ratio of ball-type metal powder.
Embodiment 1
2014 Al alloy powders (4.5wt.%Cu, 0.8wt.%Mg, 0.6wt.%Si) that particle size is 15 μm are put into ball milling
In machine, the stearic acid of 2wt.% is added as process control agent, liquid nitrogen and argon gas are passed through, in revolving speed 400rpm and ratio of grinding media to material 20:1
Ball milling parameter under ball milling 10h, obtain 2014 Al alloy powders of sheet;The flakelike powder is added in ethanol solution, is stirred
It mixes uniformly;5vol% carbon nanotube (diameter 30-50nm, 1 μm of length or so) is added in ethyl alcohol, is surpassed again after mechanical stirring 1h
Sound disperses 2h;Sheet Al powder suspension is added dropwise in carbon nano tube suspension, re-ultrasonic dispersion 1h, after filtering, drying
The composite powder on sheet Al powder surface is uniformly distributed in carbon nanotube;By the carbon nanotube of 30vol%/sheet Al composite powder
End with 20 μm of average particle size particle size, spherical morphology 2014 Al alloy powders under the parameter of revolving speed 80rpm and ratio of grinding media to material 5:1 ball
Consume time 6h, prepares final composite powder;Then, it obtains rich carbon by cold pressing, semisolid partial remelting, thixotropic forming and receives
The hierarchical structure aluminum matrix composite of the hard phase region enhancing of mitron.
Embodiment 2
The AZ91D magnesium alloy powder (9.5wt.%Al, 0.3wt.%Mn, 0.5wt.%Zn) that particle size is 35 μm is put into ball
In grinding machine, the liquid paraffin of 2wt.% is added as process control agent, liquid nitrogen and argon gas are passed through, in revolving speed 480rpm and ratio of grinding media to material
Ball milling 13h under the ball milling parameter of 20:1 obtains the AZ91D magnesium alloy powder of sheet;The flakelike powder is added to ethanol solution
In, it stirs evenly;4vol% graphene (with a thickness of 2-15nm, 2 μm of length or so) is added in ethyl alcohol, after mechanical stirring 1h again
Ultrasonic disperse 2h;Sheet magnesium dust suspension is added dropwise in graphene suspension, re-ultrasonic dispersion 1.5h, after filtering, drying
Obtain the composite powder that graphene uniform is distributed in sheet magnesium dust surface;By the graphene of 30vol%/sheet magnesium composite powder
With 50 μm of average particle size particle size, spherical morphology AZ91D magnesium alloy powder under the parameter of revolving speed 120rpm and ratio of grinding media to material 5:1 ball
Consume time 4h, prepares final composite powder;Then, rich graphite is obtained by cold pressing, semisolid partial remelting, thixotropic forming
The hierarchical structure AZ91D magnesium-based composite material of the hard phase region enhancing of alkene.
Embodiment 3
The ZA27 Zinc alloy powder (27Al-1.8Cu-0.03Mg (wt%)) that particle size is 50 μm is put into ball mill, is added
Enter the stearic acid of 2wt.% as process control agent, be passed through liquid nitrogen and argon gas, joins in the ball milling of revolving speed 380rpm and ratio of grinding media to material 20:1
Several lower ball milling 10h, obtain the ZA27 Zinc alloy powder of sheet;The flakelike powder is added in ethanol solution, is stirred evenly;It will
6vol% carbon nano-fiber (diameter 150nm, 4 μm of length or so) is added in ethyl alcohol, re-ultrasonic dispersion after mechanical stirring 0.5h
1.5h;Sheet ZA27 zinc powder suspension is added dropwise in carbon fiber suspension, re-ultrasonic dispersion 1h, obtains after filtering, drying
Carbon fiber is uniformly distributed in the composite powder on zinc flake end surface;By the carbon fiber of 25vol%/sheet zinc composite powder and put down
Equal 90 μm of particle size, spherical morphology ZA27 Zinc alloy powder under the parameter of revolving speed 80rpm and ratio of grinding media to material 5:1 Ball-milling Time
6h prepares final composite powder;Then, the hard phase of rich carbon fiber is obtained by cold pressing, semisolid partial remelting, thixotropic forming
The hierarchical Z A27 Zinc-base compounded material of area's enhancing.
Embodiment 4
For 2024 aluminium alloy preparation steps of hierarchical structure graphene nanometer sheet (GNPs) enhancing are as follows: 1) by 2024Al alloyed powder
Powder is mixed in planetary ball mill high-energy ball milling in end, obtains the flakelike powder of certain thickness and size, ball milling parameter are as follows: revolving speed
400rpm, Ball-milling Time 10h, ratio of grinding media to material 20:1, process control agent stearic acid 2wt.%, cooling medium is liquid nitrogen, and protective gas is
Argon gas.By the Al powder of sheet and 5vol%GNPs, mechanical stirring and ultrasonic disperse, filtering obtain GNPs after drying in ethanol
Uniform adsorption is in the GNPs/2024Al composite powder on sheet Al powder surface;2) by 25vol% sheet GNPs/2024Al composite powder
It is last to mix powder with spherical 2024Al alloy powder low energy ball milling, it obtains sheet GNPs/2024Al composite powder and is distributed in ball milling
(GNPs/2024Al)/2024Al mixed-powder around 2024Al powder, ball milling parameter are as follows: revolving speed 100rpm, Ball-milling Time
5h, ratio of grinding media to material 5:1, protective atmosphere are argon gas;3) pressure of (the GNPs/2024Al)/2024Al mixed-powder of 100g in 200MPa
Cold-press moulding under power obtains mixed-powder briquetting;4) mixed-powder briquetting is after 620 DEG C of semi-solid temperatures heat 60min,
Thixotropic forming under 126MPa forming pressure, 250 DEG C of mold temperatures, obtains the GNPs/2024Al composite material of hierarchical structure.
Claims (9)
1. a kind of preparation method of high tough hierarchical structure metal-base composites, which is characterized in that specific step is as follows:
(1) in liquid nitrogen cooling and under protective atmosphere, matrix alloy powder is passed through into high-energy ball milling, obtains flaky metal powder;
(2) by reinforcement, mechanical stirring and ultrasonic disperse in dispersion liquid are mixed with gained flaky metal powder, after filtering, drying
Reinforcement uniform adsorption is obtained in the composite powder I on flaky metal powder surface;
(3) again with pellet base alloy powder low energy ball milling, acquisition composite powder I is uniformly distributed in spherical gained composite powder I
Composite powder II around metal powder;
(4) gained composite powder II cold-press moulding under stress, obtains mixed-powder briquetting;
(5) gained mixed-powder briquetting heats under semi-solid temperature, obtains the semisolid non-dendritic ingot for being suitble to thixotropic forming;
(6) gained semisolid non-dendritic ingot thixotropic forming under corresponding mold temperature, forming pressure, pressure head rate, obtains
Hierarchical structure composite material.
2. preparation method according to claim 1, which is characterized in that described matrix alloy powder is Al alloy powder, magnesium
One of alloy powder, kirsite, described matrix alloy powder average grain diameter is between 3 ~ 80 μm.
3. preparation method according to claim 1, which is characterized in that the reinforcement is graphene, carbon nanotube, carbon fiber
One of dimension;Wherein, graphene size: with a thickness of 1 ~ 30nm, 1 ~ 20um of length;Carbon nanotube sizes: 20 ~ 100nm of diameter,
1 ~ 50um of length;Carbon fiber size are as follows: diameter be 50 ~ 180nm, 1 ~ 20 μm of length.
4. preparation method according to claim 1, which is characterized in that the dispersion liquid be methanol, acetone, ethyl alcohol, go from
One of sub- water, polyvinyl alcohol.
5. preparation method according to claim 1, which is characterized in that in step (1) high-energy ball milling condition be revolving speed 350 ~
500rpm, 8 ~ 14h of Ball-milling Time, ratio of grinding media to material 20:1, process control agent stearic acid 2wt.%, cooling medium are liquid nitrogen, protective gas
For argon gas.
6. preparation method according to claim 1, which is characterized in that in step (3) low energy ball milling parameter be revolving speed 80 ~
150rpm, 4 ~ 7h of Ball-milling Time, ratio of grinding media to material 5:1, protective atmosphere are argon gas.
7. preparation method according to claim 1, which is characterized in that the volume ratio of the reinforcement and flaky metal powder
For 1:10 ~ 30.
8. preparation method according to claim 1, which is characterized in that the composite powder I again with ball-type metal powder
Volume ratio is 1:2 ~ 6.
9. preparation method according to claim 1, which is characterized in that repeat step (5) ~ (6), different tissues can be prepared
The composite material of configuration.
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