CN106636708A - Method for preparing nano intermetallic compound particles and application of particles - Google Patents

Method for preparing nano intermetallic compound particles and application of particles Download PDF

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Publication number
CN106636708A
CN106636708A CN201610837260.3A CN201610837260A CN106636708A CN 106636708 A CN106636708 A CN 106636708A CN 201610837260 A CN201610837260 A CN 201610837260A CN 106636708 A CN106636708 A CN 106636708A
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ball
granule
powder
intermetallic compound
composite
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徐宏
张文达
任霁萍
杨晶
党惊知
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North University of China
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North University of China
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/047Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/142Thermal or thermo-mechanical treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/026Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Abstract

The invention relates to a method for preparing nano intermetallic compound particles and a method for applying prepared gold nanoparticles to a reinforced aluminum-based composite, provides a method for preparing a nano intermetallic compound particle reinforced aluminum-based composite, and focuses on the way of preparation of the nanoscale intermetallic compound particles. According to the basic scheme, ball-milled powder is subjected to heat treatment to form a brittle Al3M intermetallic compound, then ball milling is performed continuously, and the size is further reduced to the nanoscale; then a dispersing agent is added for dispersion and addition to melt for preparation of an aluminum-based composite; the size of the obtained reinforced intermetallic compound particles is more uniform and is smaller than or equal to 100 nm; and the reinforced particles in a matrix are dispersed more uniformly, so that the reinforced particles enter the melt more easily, and the advantage is huge in the aspect of preparation of an intermetallic compound particle reinforced metal-based composite with the high volume fraction.

Description

A kind of method for preparing nanocrystalline intermetallics granule and its application
Technical field
The present invention relates to chemical combination between a kind of method for preparing nanocrystalline intermetallics granule, and the nano metal for preparing The method that composition granule is applied to reinforced aluminum matrix composites, belongs to aluminum matrix composite and prepares and Metal Melting process technology neck Domain.
Background technology
At present, the preparation technology and method of particles reiforced metal-base composition is mainly powder metallurgic method, extrusion casint Method, spray deposition, molten liquid forming, in-situ reaction and stirring casting method.Powder metallurgic method be enhancing granule with it is fine Pure metal dust is carried out after mechanical mixture, is suppressed in a mold, and then heating is sintered, and makes enhancing phase and Metal Substrate Body assembles integral, the method for making enhancing granule/metallic composite.Stirring casting method is made by mechanical agitation enhancing Grain is added in metal bath, and is allowed to the finely dispersed method in metallic matrix.Stirring casting method equipment is simple, production effect Rate is high, but due between reinforcement and aluminum melt wettability it is poor, stir the moistening that can not improve between reinforcement and aluminum melt Property, therefore bleb is more, distribution of particles is uneven, easily forms segregation.In-situ authigenic reaction particles are in situ in intrinsic silicon Synthesis, basal body interface is combined and clean interfaces;The In-sltu reinforcement granule of variety classes, varying number can be obtained, strengthens granule Fabricated in situ combine simple process, low cost with casting, but the method has prepared composite quality point Number is not high.
Find by prior art documents, Chinese Patent Application No.:200910239051.9, publication date is 2011.06.29, the patent of the preparation method of entitled aluminum matrix composite is adopted and for nano-ceramic particle to be added to half admittedly The mixed slurry that liquid obtains liquid is warmed up to after stirring in state aluminium based metal melt, then aluminum is obtained using cast after supersound process Based composites.A kind of rich Al intermetallic reinforced aluminum matrix composites preparation method of patent (CN201310730267.1), the composite metal powder after ball milling is directly added into or is converted into after intermetallic compound particle directly In connecing addition aluminium alloy melt, can obtain that interface is good, the aluminum matrix composite of good mechanical performance.Due to metal dust Jing Surface is inevitably present oxide-film after ball milling, affects the wettability between composite powder and melt, patent:Between a kind of metal Compound particle Al3The preparation method of-M reinforced aluminum matrix composites(ZL201310730115.1)Propose a kind of using ball milling work Skill prepares the rich Al intermetallic Al of submicron order3M particle enhanced aluminum-based composite material preparation methoies, the method is adopted divides The leading method for improving magnesium density addition intermetallic compound particle in aluminum melt of step is extraordinary to solve intermetallic compound Strengthen granule and the nonwettable problem of molten metal, the engine housing composite prepared under conventional smelting temperature has good Good interface and mechanical property.Because the powder of aluminium powder and metal M is all essential plasticity, first can crack in mechanical milling process, Then can crush, as the prolongation of Ball-milling Time will continue cold welding, powder thickness is thinning, powder morphology is changed into flake, put down Face area becomes big, it will usually adds stearic acid, is beneficial to reduction cold welding, prevents powder and powder, the adhesion of powder and ball, but will not prevent The sheet trend of powder.Therefore, plastic metal powder is difficult the granule for obtaining granule even size by ball milling.And it is multiple Add after two kinds of metal dusts only ball milling after conjunction among melt, reaction is generated really under the high temperature action of solution strengthens Granule, i.e., nano level powder can continue during the course of the reaction to grow up, the enhancing granule of the aluminum matrix composite for finally giving No longer it is just nanoscale, but submicron-scale or micro-meter scale, composite powder ball milling is not just had into nanoscale yet Practical significance.
The content of the invention
The present invention overcomes the deficiencies in the prior art, technical problem to be solved to be to provide one kind and prepare change between nano metal The preparation method of polymer beads reinforced aluminum matrix composites, it is important that how to prepare the intermetallic compound particle of nanoscale.
The basic scheme of solve problem is:It is allowed to generate the Al of fragility by carrying out the powder after ball milling heat treatment3M Intermetallic compound, then proceeding to ball milling makes its size be further reduced to nanoscale;Add dispersant addition again molten Aluminum matrix composite is prepared in body.
Specifically, the technical solution adopted in the present invention is:A kind of method for preparing nanocrystalline intermetallics granule, bag Include following steps:
(1)By aluminium powder and metal M powder in molar ratio 3:1 is configured to composite powder, under vacuum ball milling, rotational speed of ball-mill 300- 500r/min, Ball-milling Time 10-20h, ratio of grinding media to material 10-20:1;
(2)The good composite powder of ball milling heat treatment 0.5-2h at 400-550 DEG C in a vacuum furnace, makes composite powder reaction generate fragility Intermetallic compound Al3M, rear furnace cooling;
(3)By Jing steps(2)Intermetallic compound after heat treatment further ball milling under argon protective condition is reached to be received Metrical scale, rotational speed of ball-mill 300-500r/min, Ball-milling Time 10-20h, ratio of grinding media to material 10-20:1, obtain nanocrystalline intermetallics Granule.
Heretofore described metal M, M are the one kind in titanium, zirconium, ferrum, scandium or erbium.
Before already explained above aluminium powder and metal M powder belong to plastic metal powder, it is desirable to obtain the granule of nanoscale, no Only ball milling difficulty is big(Need high ratio of grinding media to material and longer Ball-milling Time, and the auxiliary agent such as stearic acid)Even if, and received The granule of metrical scale, it is also difficult to ensure the uniformity of yardstick.Therefore, typically to obtain nanometer aluminium powder is will not to adopt simple machine Tool ball milling, it is typically with the methods such as evaporative condenser, mechanochemistry, laser ablation.
According to nanocrystalline intermetallics granule prepared by the method for the present invention, the enhancing of aluminum matrix composite is can serve as The matrix of body, wherein aluminum and composite can make aluminum, or aluminium alloy.
The method for specifically preparing aluminum matrix composite, can be according to following steps:
(1)By nanocrystalline intermetallics granule and matrix material in mass ratio 1:1-4 dispensings, are mixed using ball milling method Close, make nanocrystalline intermetallics granule dispersed in matrix material, obtain composite powder;Described matrix material is aluminium powder Or Al alloy powder.
The purpose of ball milling is that nanocrystalline intermetallics granule is pre-dispersed in matrix material in this step, is added In matrix melt, could be scattered more uniform;The condition of ball milling can voluntarily determine according to experiment, or according to following bar Part:50 ~ 100r/min of rotational speed of ball-mill, Ball-milling Time 5-10h, ratio of grinding media to material 5:1~10:1.
Wherein step(1)The material of the Al alloy powder for being used should be identical with the material of the matrix solution of next step.
(2)By step(1)The composite powder for obtaining adds the matrix for being superheated to 800-850 DEG C in the form of powdery or bulk It is stirring while adding in melt, 10-30min is stirred altogether;
(3)Temperature is adjusted after final refined, standing to pouring temperature 690-710 DEG C, casting obtains intermetallic compound Al3-M The enhanced aluminum matrix composite of granule.
In the present invention, the aluminium alloy that matrix is selected can be alusil alloy, aluminium copper, almag, alumin(i)um zinc alloy and Al rare earth alloy, wherein the matrix material of dispersion nanocrystalline intermetallics granule is and the same material of the matrices of composite material to be prepared The alloy powder of matter.
Particle enhanced aluminum-based composite material prepared according to the methods of the invention, the intermetallic compound Al3- M granules Size≤100nm, can effectively hinder dislocation motion, play invigoration effect.
Heretofore described matrices of composite material alloy powder is referred to when the base of aluminum matrix composite to be prepared When body is aluminium alloy, with the same material of the matrix phase of aluminum matrix composite to be prepared.
Compared with prior art the invention has the advantages that.
The reinforcement intermetallic compound particle size of acquisition is more uniform, and size≤100nm;Strengthen granule in matrix Dispersion is more uniform, makes enhancing granule be easier to enter melt, strengthens in the intermetallic compound particle for preparing high-volume fractional Metal-base composites aspect, with very big advantage.The intermetallic compound particle of the nanoscale of preparation is directly added into In melt, it is to avoid composite powder directly adds the problem of the particle growth that reaction is caused, it is ensured that the grain of the reinforcement of composite Degree asks Nano grade.
The proportioning of intermetallic compound and matrix, metalwork compound can more neatly be changed using the method for the present invention Content can change in the range of at least 0.5-5wt%, be obtained higher volume fraction Al3- M intermetallic compounds-metal Based composites, and improve Al3Degree of scatter of-M the intermetallic compounds in metallic matrix.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of method for preparing nanocrystalline intermetallics granule, comprises the following steps:
(1)By aluminium powder and metal M powder in molar ratio 3:1 is configured to composite powder, under vacuum ball milling, rotational speed of ball-mill 500r/ Min, Ball-milling Time 20h, ratio of grinding media to material 10:1;
(2)The good composite powder of ball milling heat treatment 1.5h at 400 DEG C in a vacuum furnace, makes composite powder reaction generate between brittle metal Compound Al3M, rear furnace cooling;
(3)By Jing steps(2)Intermetallic compound after heat treatment further ball milling under argon protective condition is reached to be received Metrical scale, rotational speed of ball-mill 350r/min, Ball-milling Time 15h, ratio of grinding media to material 16:1, obtain nanocrystalline intermetallics granule.
Embodiment 2
A kind of method for preparing nanocrystalline intermetallics granule, comprises the following steps:
(1)By aluminium powder and metal M powder in molar ratio 3:1 is configured to composite powder, under vacuum ball milling, rotational speed of ball-mill 300r/ Min, Ball-milling Time 14h, ratio of grinding media to material 15:1;
(2)The good composite powder of ball milling heat treatment 2h at 450 DEG C in a vacuum furnace, makes composite powder reaction generate between brittle metal and changes Compound Al3M, rear furnace cooling;
(3)By Jing steps(2)Intermetallic compound after heat treatment further ball milling under argon protective condition is reached to be received Metrical scale, rotational speed of ball-mill 500r/min, Ball-milling Time 18h, ratio of grinding media to material 15:1, obtain nanocrystalline intermetallics granule.
Embodiment 3
A kind of method for preparing nanocrystalline intermetallics granule, comprises the following steps:
(1)By aluminium powder and metal M powder in molar ratio 3:1 is configured to composite powder, under vacuum ball milling, rotational speed of ball-mill 450r/ Min, Ball-milling Time 10h, ratio of grinding media to material 20:1;
(2)The good composite powder of ball milling heat treatment 1h at 500 DEG C in a vacuum furnace, makes composite powder reaction generate between brittle metal and changes Compound Al3M, rear furnace cooling;
(3)By Jing steps(2)Intermetallic compound after heat treatment further ball milling under argon protective condition is reached to be received Metrical scale, rotational speed of ball-mill 300r/min, Ball-milling Time 20h, ratio of grinding media to material 10:1, obtain nanocrystalline intermetallics granule.
Embodiment 4
A kind of method for preparing nanocrystalline intermetallics granule, comprises the following steps:
(1)By aluminium powder and metal M powder in molar ratio 3:1 is configured to composite powder, under vacuum ball milling, rotational speed of ball-mill 380r/ Min, Ball-milling Time 15h, ratio of grinding media to material 10-20:1;
(2)The good composite powder of ball milling heat treatment 0.5h at 550 DEG C in a vacuum furnace, makes composite powder reaction generate between brittle metal Compound Al3M, rear furnace cooling;
(3)By Jing steps(2)Intermetallic compound after heat treatment further ball milling under argon protective condition is reached to be received Metrical scale, rotational speed of ball-mill 400r/min, Ball-milling Time 10h, ratio of grinding media to material 20:1, obtain nanocrystalline intermetallics granule.
Embodiment 5
The method for preparing aluminum matrix composite, can be according to following steps:
(1)Nanocrystalline intermetallics granule prepared by embodiment 1 and aluminium powder in mass ratio 1:1 dispensing, using ball milling method Mixed, make nanocrystalline intermetallics granule dispersed in matrix material, obtained composite powder;
(2)By step(1)The composite powder for obtaining is added in the form of powdery or bulk and is superheated in 800 DEG C of matrix melt, It is stirring while adding, 20min is stirred altogether;
(3)Temperature is adjusted after final refined, standing to pouring temperature 690-710 DEG C, casting obtains intermetallic compound Al3-M The enhanced aluminum matrix composite of granule.
Embodiment 6
The method for preparing aluminum matrix composite, can be according to following steps:
(1)Nanocrystalline intermetallics granule prepared by embodiment 2 and alusil alloy powder in mass ratio 1:2 dispensings, adopt Ball milling method is mixed, and makes nanocrystalline intermetallics granule dispersed in matrix material, obtains composite powder;
50 ~ 100r/min of rotational speed of ball-mill, Ball-milling Time 5-10h, ratio of grinding media to material 8:1;
(2)By step(1)The composite powder for obtaining is added in the form of powdery or bulk and is superheated in 850 DEG C of matrix melt, It is stirring while adding, 25min is stirred altogether;
(3)Temperature is adjusted after final refined, standing to pouring temperature 690-710 DEG C, casting obtains intermetallic compound Al3-M The enhanced aluminum matrix composite of granule.
Embodiment 7
The method for preparing aluminum matrix composite, can be according to following steps:
(1)Nanocrystalline intermetallics granule prepared by embodiment 3 and aluminium copper powder in mass ratio 1:3 dispensings, adopt Ball milling method is mixed, and makes nanocrystalline intermetallics granule dispersed in matrix material, obtains composite powder;
50 ~ 100r/min of rotational speed of ball-mill, Ball-milling Time 5-10h, ratio of grinding media to material 10:1;
(2)By step(1)The composite powder for obtaining is added in the form of powdery or bulk and is superheated in 833 DEG C of matrix melt, It is stirring while adding, 30min is stirred altogether;
(3)Temperature is adjusted after final refined, standing to pouring temperature 690-710 DEG C, casting obtains intermetallic compound Al3-M The enhanced aluminum matrix composite of granule.
Embodiment 8
The method for preparing aluminum matrix composite, can be according to following steps:
(1)Nanocrystalline intermetallics granule prepared by embodiment 4 and al-mg alloy powder in mass ratio 1:4 dispensings, adopt Ball milling method is mixed, and makes nanocrystalline intermetallics granule dispersed in matrix material, obtains composite powder;
50 ~ 100r/min of rotational speed of ball-mill, Ball-milling Time 5-10h, ratio of grinding media to material 5:1;
(2)By step(1)The composite powder for obtaining is added in the form of powdery or bulk and is superheated in 840 DEG C of matrix melt, It is stirring while adding, 10min is stirred altogether;
(3)Temperature is adjusted after final refined, standing to pouring temperature 690-710 DEG C, casting obtains intermetallic compound Al3-M The enhanced aluminum matrix composite of granule.
The present invention can be summarized with others without prejudice to the concrete form of the spirit or essential characteristics of the present invention.Therefore, nothing By from the point of view of which point, the embodiment above of the present invention can only all be considered the description of the invention and can not limit invention, Claims indicate the scope of the present invention, and the scope of the present invention is not pointed out in above-mentioned explanation, therefore, with the present invention The suitable implication and scope of claims in any change, be all considered as being included within the scope of the claims.

Claims (4)

1. a kind of method for preparing nanocrystalline intermetallics granule, it is characterised in that comprise the following steps:
(1)By aluminium powder and metal M powder in molar ratio 3:1 is configured to composite powder, under vacuum ball milling, rotational speed of ball-mill 300- 500r/min, Ball-milling Time 10-20h, ratio of grinding media to material 10-20:1;The M is the one kind in titanium, zirconium, ferrum, scandium or erbium;
(2)The good composite powder of ball milling heat treatment 0.5-2h at 400-550 DEG C in a vacuum furnace, makes composite powder reaction generate fragility Intermetallic compound Al3- M, rear furnace cooling;
(3)By Jing steps(2)Intermetallic compound after heat treatment further ball milling under argon protective condition is reached to be received Metrical scale, rotational speed of ball-mill 300-500r/min, Ball-milling Time 10-20h, ratio of grinding media to material 10-20:1, obtain nanocrystalline intermetallics Granule.
2. the nanocrystalline intermetallics granule that prepared by method according to claim 1, it is characterised in that:The nanometer gold Application of the compound particle in aluminum matrix composite is prepared between category, the matrix of the aluminum matrix composite is aluminum or aluminum alloy, Reinforcement is nanocrystalline intermetallics granule.
3. nanocrystalline intermetallics granule according to claim 2, it is characterised in that prepare aluminium base by following steps Composite:
(1)By nanocrystalline intermetallics granule and matrix material in mass ratio 1:1-4 dispensings, are mixed using ball milling method Close, make nanocrystalline intermetallics granule dispersed in matrix material, obtain composite powder;Described matrix material is aluminium powder Or Al alloy powder;
(2)By step(1)The composite powder for obtaining adds the matrix melt for being superheated to 800-850 DEG C in the form of powdery or bulk In, it is stirring while adding, 10-30min is stirred altogether;
(3)Temperature is adjusted after final refined, standing to pouring temperature 690-710 DEG C, casting obtains intermetallic compound Al3-M The enhanced aluminum matrix composite of granule.
4. nanocrystalline intermetallics granule according to claim 3, it is characterised in that:Step(1)Ball milling condition be: 50 ~ 100r/min of rotational speed of ball-mill, Ball-milling Time 5-10h, ratio of grinding media to material 5:1~10:1.
CN201610837260.3A 2016-09-21 2016-09-21 Method for preparing nano intermetallic compound particles and application of particles Pending CN106636708A (en)

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CN113215444A (en) * 2021-04-23 2021-08-06 广东省科学院材料与加工研究所 Nano-particle reinforced TC4 metal powder material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN112893851A (en) * 2021-01-16 2021-06-04 昆明理工大学 Method for directly preparing copper-aluminum intermetallic compound powder by mechanical alloying
CN112893851B (en) * 2021-01-16 2023-02-24 昆明理工大学 Method for directly preparing copper-aluminum intermetallic compound powder by mechanical alloying
CN113215444A (en) * 2021-04-23 2021-08-06 广东省科学院材料与加工研究所 Nano-particle reinforced TC4 metal powder material and preparation method thereof

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Application publication date: 20170510