CN107262729B - A kind of preparation method of the equally distributed particulate reinforced metal-based complex spherical powder material of reinforced phase - Google Patents
A kind of preparation method of the equally distributed particulate reinforced metal-based complex spherical powder material of reinforced phase Download PDFInfo
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- CN107262729B CN107262729B CN201710537878.2A CN201710537878A CN107262729B CN 107262729 B CN107262729 B CN 107262729B CN 201710537878 A CN201710537878 A CN 201710537878A CN 107262729 B CN107262729 B CN 107262729B
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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
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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Abstract
The invention discloses a kind of preparation methods of the equally distributed particulate reinforced metal-based complex spherical powder material of reinforced phase, after this method carries out mechanical mixture using metal powder and reinforced phase powder, it is formed and is sintered by PM technique and composite bar is made, the equally distributed particulate reinforced metal-based complex spherical powder material of reinforced phase is made using no crucible for smelting aerosolization technology in composite bar, the composite powder impurity of this method preparation is few, hardening constituent is uniformly distributed, powder is spherical or subsphaeroidal, with excellent mobility and high apparent density, as powder metallurgy, injection moulding, the raw material of the technologies such as 3D printing, with unique advantage and irreplaceability, the device of excellent combination property can be obtained.
Description
Technical field
The present invention relates to the preparation of metal powder material, in particular to a kind of reinforced phase with spherical or subsphaeroidal shape
The preparation method of equally distributed particulate reinforced metal-based composite powder material, belongs to powder metallurgical technology.
Background technique
Metal-base composites can overcome certain limitations of homogenous material compared with traditional metal materials, realize collaboration effect
It answers, has many advantages, such as higher specific strength, specific modulus and heat resistance.Due to enhancing particle have it is from a wealth of sources, cheap and
The advantages that preparation process is relatively easy, therefore particles reiforced metal-base composition is most widely used, is applied to aviation
The fields such as space flight, military and national defense and nuclear industry.The grain reinforced metal composite material for having obtained industrial application at present has carbonization
Titanium enhances titanium alloy, SiC reinforcement aluminium alloy etc..
The preparation method of particles reiforced metal-base composition mainly has powder metallurgic method, casting and in-situ compositing
Deng.In recent years, increases material manufacturing technology becomes the research hotspot for preparing composite material.Metal increases material manufacturing technology is based on layering system
Make principle, by successively preparing, accumulation superposition molded samples, have plastic complex parts, be designed into it is with short production cycle and
Without particular advantages such as molds.It is well known that metal increases material manufacturing technology is both needed to powder with certain mobility, to guarantee to send
The high density of powder/powdering uniformity and bisque of mating formation.When using mixed-powder as raw material, because of metal powder and reinforced phase
Powder diameter and density difference are larger and generate the non-uniform phenomenons such as layering, and reinforced phase is caused to be unevenly distributed or reinforced phase additional amount
It can not accurately regulate and control, and reinforced phase grain shape is generally irregular, and granularity is tiny, will lead to the flowing of mixed-powder
Property is poor.
Chinese patent CN105583401A discloses the preparation method of composite powder for 3D printing a kind of, product and answers
With, metal powder and ceramic powders are subjected to high-energy ball milling, are uniformly mixed reinforced phase with parent metal using high-energy ball milling, from
And composite powder is prepared, it can be used for metal increasing material manufacturing.It is high although the available uniformly mixed composite powder of this method
Energy ball milling will change the pattern of powder, cannot get spherical powder, thus the mobility of powder can be lost, and high-energy ball milling can also
The pollution of ball-milling medium is introduced, the purity of powder cannot be guaranteed.Chinese patent CN106363185A discloses another kind and is used for
The method for preparing powder metallurgy of composite powder and its block materials, by nano-phase powder end, the low speed of metal powder elder generation through a long time
Ball milling makes metal powder tailpiece, and nanometer is made mutually to be dispersed in the surface or inside of piece metal powder simultaneously, obtains nanometer
Phase/Metal Flake composite powder；Again through high speed ball milling in short-term, makes a nanometer phase/Metal Flake composite powder soldering, obtain nanometer
Phase/metallic particles shape composite powder；Although this method can solve nanometer phase in metallic matrix by adjusting ball milling speed
Evenly dispersed and interface cohesion problem, but its spherical powder that can not obtain good fluidity.Therefore, prior art preparation is answered
Closing powder is irregular shape, poor fluidity, and easily introducing clast impurity, influences purity.
Existing aerosolization technology is mainly used to prepare metal powder material, and can prepare spherical shape under certain conditions
Or subsphaeroidal metal powder material, there is excellent mobility and high apparent density, be highly suitable for increasing material manufacturing
It is required that.And existing gas atomization existing the biggest problem when preparing metal powder is, centre is poured into after by metal molten
During metal liquid is introduced atomization chamber by Bao Bingjing diversion pipe, since ceramic enhancement phase is compared with the wetability of metal liquid
Difference directly makes an addition to enhancing particle inside metal bath, and reinforced phase can assemble and float on the surface of melt, cannot achieve enhancing
Mutually being uniformly distributed in metal_based material；Meanwhile the viscosity of such compounding flux will increase very much, it is also difficult to realize gas
It is atomized the requirement to metal bath mobility, therefore is difficult to prepare the equally distributed particle of reinforced phase using conventional gas atomization
Enhance metal-based compound powder body material.
In conclusion the particulate reinforced metal-based composite powder material prepared in the prior art can not have both good fluidity,
The advantages that purity is high and reinforced phase are uniformly distributed.
Summary of the invention
For existing particulate reinforced metal-based composite powder material there are poor fluidity, purity is low the problems such as, and it is existing
Aerosolization technology be difficult to prepare the defect of the equally distributed metal-based compound powder of reinforced phase, the purpose of the present invention is be to mention
It is uniformly distributed in single metal powder for a kind of reinforced phase, and pattern is that standard is spherical or subsphaeroidal, has good fluidity
High purity granular enhancing metal-based compound powder body material preparation method, overcome existing high-energy ball milling powder poor fluidity,
The technical problem of the equally distributed metal-based compound powder of reinforced phase can not be prepared by being easily introduced impurity pollution and conventional gas atomization.
In order to achieve the above technical purposes, it is equally distributed particulate reinforced metal-based multiple that the present invention provides a kind of reinforced phases
The preparation method of spherical powder material is closed, this method is by metal powder and reinforced phase powder using V-type batch mixer or low energy ball
After mill mixing, composite bar is prepared by powder metallurgic method molding and sintering；The composite bar utilizes no crucible induction melting
Gas atomization equipment prepares particulate reinforced metal-based complex spherical powder material；The no crucible induction melting gas atomization equipment
Charging rate be 10mm/min~160mm/min, atomizing pressure be 1.0MPa~10.0MPa, atomizing medium be argon gas, helium
Gas, hydrogen or nitrogen.
More preferably scheme, the metal powder include one or both of iron-based, Ni-based, aluminium base, copper-based, titanium-based with
On element powders or alloy powder.
Preferred scheme, reinforced phase powder are within reinforced phase powder and the 20% of metal powder gross mass；More preferably
Within 5%.
Preferred scheme, the charging rate of the no crucible induction melting gas atomization equipment are 20mm/min~100mm/
Min, atomizing pressure are 2.0MPa~8.0MPa.
Further preferred scheme, the partial size of the metal powder are 1~500 μm.
More preferably scheme, the reinforced phase powder includes TiC, Al2O3, at least one of WC, SiC, TiN or C and/
Or B4C, wherein C and B4C mainly generates reinforced phase by reacting with metallic element.
Further preferred scheme, the partial size of the reinforced phase powder are 1nm~10 μm.
Preferred scheme aoxidizes in order to prevent during V-type batch mixer or low energy ball milling mixing, can be in mixing
Protective gas, such as inert gas are filled in device.
Preferred scheme, the powder metallurgic method include hot pressing, molding-sintering, isostatic cool pressing-sintering or hot isostatic pressing.
More preferably scheme, in order to reach preferable electrode sensing requirement, the relative density of composite bar (actual density with
The ratio of theoretical density) it is preferably up to 95% or more.
Preferred scheme, the diameter of the composite bar are 30~150mm.
Preferred scheme, the particulate reinforced metal-based complex spherical powder material of preparation is according to application demand, using routine
Method be classified (such as sieve method or air current classifying), choosing required particle size range powder can be used to PM technique
Composite material is prepared with 3D printing technique.
Existing particulate reinforced metal-based composite powder material has that poor fluidity, impurity content are high, and existing
Although aerosolization technology can prepare the metal powder material of good fluidity, exist to be difficult to prepare reinforced phase and be uniformly distributed
Metal Substrate reinforced phase composite powder defect.Present invention firstly provides use simple and mechanical mixing+powder metallurgic method molding+nothing
Crucible induction melting Gas atomization techniques prepare the group technology of powder, successfully prepare reinforced phase and are uniformly distributed, and mobility
Good, with high purity particulate reinforced metal-based composite powder material.It is simple by V-type batch mixer or using low energy ball milling etc. first
Mechanical mixture technique the mixing of powder raw material may be implemented, and can be polluted to avoid powder in high-energy ball milling mixed process.?
On the basis of this, mixed-powder is shaped and is sintered to compound using the conventional powder metallurgic method such as technologies such as powder cold pressing or hot pressing
Bar overcomes conventional melting that reinforced phase is caused to separate or the shortcomings that be unevenly distributed.The present invention is further incuded using no crucible
Melting Gas atomization techniques carry out powder by atomization, by using no crucible induction melting gas atomization equipment, since it is without in
Between packet and diversion pipe, it can be achieved that high viscosity metal bath prepares powder body material, can effectively avoid melting in composite granule raw material
Reinforced phase is precipitated in molten matrix metal in the process, to obtain enhancing even particle distribution, shape is spherical in shape and subsphaeroidal,
With good mobility and high apparent density, it is highly suitable for powder metallurgy and 3D printing increasing material manufacturing raw material.
The present invention use without crucible electrode induction melting gas atomization equipment for equipment well known in the prior art.As in
State's patent (publication number CN106424748A).
Compared with the prior art, technical solution of the present invention bring advantageous effects:
1, particulate reinforced metal-based complex spherical powder material prepared by the present invention is that standard is spherical or subsphaeroidal, has stream
Dynamic property is good, the excellent feature of apparent density, and preparation process impurity introduction volume is low, can guarantee the high-purity feature of powder body material,
Meanwhile reinforced phase is evenly distributed in metallic matrix, help to obtain high-performance composite materials, be highly suitable for powder metallurgy and
3D printing increasing material manufacturing raw material.
2, particulate reinforced metal-based composite spherical powder prepared by the present invention fundamentally solves current 3D printing metal
The raw material of based composites be that poor fluidity, purity existing for mixed-powder is low and reinforced phase can not the technology of accuracy controlling ask
Topic.Meanwhile using powder prepared by the present invention as raw material, can on conventional 3D printer forming metal based composites, improve
The universality of conventional 3D printing equipment.
3, the present invention is not necessarily to high-energy ball milling during preparing particulate reinforced metal-based complex spherical powder material, can reduce
Impurity in mixed-powder introduces, while using no crucible for smelting aerosolization technology, avoiding contact of the molten metal with crucible, prepares
Powder purity it is higher.
4, the present invention is prepared during particulate reinforced metal-based complex spherical powder material to metal matrix material and increasing
The type and proportion of strong particle are alternative strong, and material designability is strong.
5, the present invention prepares the simple process of particulate reinforced metal-based complex spherical powder material, and equipment is mature, can be used for
Industrial mass production.
Detailed description of the invention
[Fig. 1] is the process flow chart of present invention preparation spherical metal base composite powder.
[Fig. 2] is no crucible for smelting aerosolizing device schematic diagram.
[Fig. 3] is spherical shape Ti6Al4V/TiC composite powder pattern prepared by the present invention.
[Fig. 4] is the distribution map of TiC in spherical shape Ti6Al4V/TiC composite powder prepared by the present invention.
Specific embodiment
Below by the present invention is described further in conjunction with the embodiments.The present embodiment is served only for saying of the invention
It is bright, it is not intended to limit to protection scope of the present invention.
Embodiment 1
It is used to prepare titanium alloy composite powder
Select partial size be 10 μm~150 μm aerosolization Ti6Al4V powder and partial size be 1.5 μm TiC powder, according to
Lower mass percent carries out ingredient: the Ti6Al4V alloy powder of 95wt.%, the TiC of 5wt.%.It will be weighed according to above-mentioned formula
Powder be placed in V-type batch mixer, to prevent powder in mixing process from aoxidizing, vacuumize, be re-filled with after mixing tank is sealed
Argon gas.Mixing revolving speed is 100rad/min, time 2h.It is to be in 35mm graphite hot pressing die that mixed-powder, which is put into diameter,
The pollution for preventing charcoal in graphite jig coats BN lubricant in mould inner wall.Sintering temperature is 1100 DEG C, pressure 16MPa, is protected
Warm time 1h, sintering atmosphere are argon gas protection.Composite bar one end after sintering is machined as to 70 ° of cone angle, surface
It is polished with sand paper.Using no crucible induction melting aerosolizing device, argon gas is atomization gas, control charging rate be 20~
The equally distributed composite powder of hardening constituent TiC can be made in 40mm/min, 3.5~8.0MPa of atomizing pressure.It is aobvious using scanning electron
Micro mirror carries out sphericity observation to powder, and powder is spherical or subsphaeroidal.
Embodiment 2
It is used to prepare titanium-based composite powder
Select the irregular pure Ti powder that partial size is 10 μm~60 μm and the B that partial size is 400nm4C powder, according to following
Mass percent carries out ingredient: the Ti powder of 98wt.%, the B of 2wt.%4C.Ball will be placed according to the weighed powder of above-mentioned formula
Grinding jar, ratio of grinding media to material 1:1, mill ball material used are 201 stainless steels.To prevent powder in mixing process from aoxidizing, by ball
It is vacuumized after grinding jar sealing, is re-filled with argon gas.Rotational speed of ball-mill is 250rad/min, Ball-milling Time 4h.Mixed-powder is put into
Diameter is the rubber package set of 50mm, is formed in isostatic cool pressing equipment, briquetting pressure 250MPa.After isostatic cool pressing
Green compact is sintered in vacuum sintering furnace, and sintering temperature is 1400 DEG C, soaking time 2h.By the composite bar after sintering
One end is machined as 60 ° of cone angle, and sand for surface paper is polished.Using no crucible induction melting aerosolizing device, (if it is
Independent research is had to) argon gas be atomization gas, control charging rate be 25~35mm/min, atomizing pressure 3.5~
The equally distributed composite powder of hardening constituent TiC and TiB can be made in 6.0MPa.Ball is carried out to powder using scanning electron microscope
The observation of shape degree, powder are spherical or subsphaeroidal.
Embodiment 3
It is used to prepare aluminium alloy compound powder
The aerosolization AlSi10Mg powder that partial size is 10 μm~150 μm and the AlN powder that partial size is 2.0 μm are selected, according to
Following mass percent carries out ingredient: the AlSi10Mg alloy powder of 96wt.%, the AlN of 4wt.%.It will claim according to above-mentioned formula
The powder taken is placed in ball grinder, ratio of grinding media to material 2:1, and mill ball material used is corundum (Al2O3).To prevent powder in mixing process
End aoxidizes, and vacuumizes after ball grinder is sealed, is re-filled with argon gas.Low energy rotational speed of ball-mill is 150rad/min, Ball-milling Time
For 1h.It is in 45mm graphite hot pressing die that mixed-powder, which is put into diameter,.Sintering temperature is 610 DEG C, pressure 12MPa, heat preservation
Time 1.5h, sintering atmosphere are argon gas protection.Composite bar one end after sintering is machined as to 120 ° of cone angle, surface
It is polished with sand paper.Using no crucible induction melting aerosolizing device, nitrogen is atomization gas, control charging rate be 30~
The equally distributed composite powder of hardening constituent AlN can be made in 50mm/min, 2.0~4.0MPa of atomizing pressure.It is aobvious using scanning electron
Micro mirror carries out sphericity observation to powder, and powder is spherical or subsphaeroidal.
Claims (6)
1. a kind of preparation method of the equally distributed particulate reinforced metal-based complex spherical powder material of reinforced phase, feature exist
In: after metal powder and reinforced phase powder are used V-type batch mixer or low energy ball milling mixing, passes through powder metallurgic method and form and burn
Knot prepares composite bar；The composite bar is prepared particulate reinforced metal-based multiple using no crucible induction melting gas atomization equipment
Close spherical powder material；The charging rate of the no crucible induction melting gas atomization equipment is 10mm/min~160mm/min,
Atomizing pressure is 1.0MPa~10.0MPa, and atomizing medium is argon gas, helium, hydrogen or nitrogen；The diameter of the composite bar is
30~150mm；Mixed-powder is 95% or more through molding and sintered composite bar relative density.
2. the preparation of the equally distributed particulate reinforced metal-based complex spherical powder material of reinforced phase according to claim 1
Method, it is characterised in that: the metal powder includes one or more of iron-based, Ni-based, aluminium base, copper-based, titanium-based
Element powders or alloy powder.
3. the preparation of the equally distributed particulate reinforced metal-based complex spherical powder material of reinforced phase according to claim 2
Method, it is characterised in that: the partial size of the metal powder is 1~500 μm.
4. the preparation of the equally distributed particulate reinforced metal-based complex spherical powder material of reinforced phase according to claim 1
Method, it is characterised in that: the reinforced phase powder includes TiC, Al2O3, WC, SiC, at least one of TiN powder, or can be with
Basic metallic element reaction generates the C and/or B of reinforced phase4C powder.
5. the equally distributed particulate reinforced metal-based complex spherical powder of reinforced phase according to any one of claims 1 to 4
The preparation method of material, it is characterised in that: the partial size of the reinforced phase powder is 1nm~10 μm.
6. the equally distributed particulate reinforced metal-based complex spherical powder of reinforced phase according to any one of claims 1 to 4
The preparation method of material, it is characterised in that: the powder metallurgic method includes hot pressing, molding-sintering, isostatic cool pressing-sintering or heat
Equal static pressure.
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