CN107262729A - It is a kind of to strengthen the preparation method of mutually equally distributed particulate reinforced metal-based complex spherical powder material - Google Patents
It is a kind of to strengthen the preparation method of mutually equally distributed particulate reinforced metal-based complex spherical powder material Download PDFInfo
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- CN107262729A CN107262729A CN201710537878.2A CN201710537878A CN107262729A CN 107262729 A CN107262729 A CN 107262729A CN 201710537878 A CN201710537878 A CN 201710537878A CN 107262729 A CN107262729 A CN 107262729A
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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
Strengthen the preparation method of mutually equally distributed particulate reinforced metal-based complex spherical powder material the invention discloses a kind of, this method is carried out after mechanical mixture using metal dust with enhancing phase powder, it is molded and is sintered by PM technique and composite bar is made, composite bar is utilized is made the mutually equally distributed particulate reinforced metal-based complex spherical powder material of enhancing without crucible for smelting aerosolization technology, composite powder impurity prepared by this method 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, more particularly to a kind of enhancing 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 technology
Metal-base composites can overcome some limitations of homogenous material compared with traditional metal materials, realize collaboration effect
Should, there is higher specific strength, specific modulus and heat resistance.Due to enhancing particle there are wide material sources, it is cheap and
The advantages of preparation technology 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.Having obtained the grain reinforced metal composite of commercial Application at present has carbonization
Titanium strengthens 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 turns into the study hotspot for preparing composite.Metal increases material manufacturing technology is based on layering system
Make principle, by successively preparing, accumulation superposition molded samples, with plastic complex partses, be designed into it is with short production cycle and
Without particular advantages such as moulds.It is well known that metal increases material manufacturing technology, which is both needed to powder, has certain mobility, to ensure to send
The high density of powder/powdering uniformity and bisque of mating formation.When using mixed-powder as raw material, because of metal dust and enhancing phase
Powder diameter and density difference are larger and produce the non-uniform phenomenons such as layering, cause enhancing distributed mutually uneven or the enhancing amount of being added to
Can not accurately it regulate and control, and it is generally irregular to strengthen phase grain shape, and granularity is tiny, can cause the flowing of mixed-powder
Property is poor.
Chinese patent CN105583401A discloses a kind of preparation method of the composite powder for 3D printing, product and answered
With, metal dust and ceramic powders are subjected to high-energy ball milling, will be strengthened using high-energy ball milling and be well mixed with parent metal, from
And composite powder is prepared, available for metal increasing material manufacturing.It is high although this method can obtain well mixed composite powder
Can ball milling will change the pattern of powder, cannot get spherical powder, thus the mobility of powder can lose, 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 be used for
The method for preparing powder metallurgy of composite powder and its block materials, by nano-phase powder end, metal dust first through prolonged low speed
Ball milling makes metal powder tailpiece, and nanometer is mutually dispersed in the surface or inside of piece metal dust simultaneously, obtains nanometer
Phase/Metal Flake composite powder；Again through high speed ball milling in short-term, make a nanometer phase/Metal Flake composite powder soldering, obtain nanometer
Phase/metallic particles shape composite powder；Although this method can solve nanometer in metallic matrix by adjusting ball milling speed
Dispersed and interface cohesion problem, but it can not obtain the spherical powder of good fluidity.Therefore, what prepared by prior art answers
It is irregular shape, poor fluidity, and easily introducing chip impurity to close powder, influences purity.
Existing aerosolization technology is mainly used to prepare metal powder material, and can prepare under certain conditions spherical
Or subsphaeroidal metal powder material, with excellent mobility and high apparent density, it is highly suitable for increasing material manufacturing
It is required that.And the biggest problem that existing gas atomization exists when preparing metal dust is, centre is poured into after by metal molten
During metal liquid to be introduced to Bao Bingjing mozzles atomization chamber, because ceramic enhancement phase is compared with the wetability of metal liquid
Difference, enhancing particle is directly made an addition to inside metal bath, and enhancing, which is met, assembles and float on the surface of melt, it is impossible to realize enhancing
Being uniformly distributed in metal_based material；Meanwhile, the viscosity of such compounding flux can increase a lot, it is also difficult to realize gas
The requirement to metal bath mobility is atomized, therefore the mutually equally distributed particle of preparation enhancing is difficult to using conventional gas atomization
Strengthen metal-based compound powder body material.
In summary, the particulate reinforced metal-based composite powder material prepared in the prior art can not have concurrently good fluidity,
The advantages of purity height is mutually uniformly distributed with enhancing.
The content of the invention
There is the low problem of poor fluidity, purity for existing particulate reinforced metal-based composite powder material, and it is existing
Aerosolization technology be difficult to the defect for preparing the mutually equally distributed metal-based compound powder of enhancing, the purpose of the present invention is to be to carry
Mutually it is uniformly distributed in single metal powder for one kind enhancing, and pattern is that standard is spherical or subsphaeroidal, with good fluidity
High purity granular strengthen metal-based compound powder body material preparation method, overcome existing high-energy ball milling powder poor fluidity,
Being easily introduced impurity pollution and can not being prepared with conventional gas atomization strengthens the technical barrier of mutually equally distributed metal-based compound powder.
In order to realize above-mentioned technical purpose, the invention provides one kind enhancing is mutually equally distributed particulate reinforced metal-based multiple
The preparation method of spherical powder material is closed, this method is using V-type batch mixer or low energy ball by metal dust with enhancing phase powder
After mill mixing, composite bar is prepared by powder metallurgic method shaping and sintering；The composite bar is utilized without crucible induction melting
Gas atomization equipment prepares particulate reinforced metal-based complex spherical powder material；It is described without 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 dust include one or both of iron-based, Ni-based, aluminium base, copper-based, titanium-based with
On element powders or alloy powder.
It is preferred that scheme, within enhancing phase powder is enhancing phase powder and the 20% of metal dust gross mass；More preferably
Within 5%.
It is preferred that scheme, the charging rate without crucible induction melting gas atomization equipment be 20mm/min~100mm/
Min, atomizing pressure is 2.0MPa~8.0MPa.
Further preferred scheme, the particle diameter of the metal dust is 1~500 μm.
More preferably scheme, the enhancing phase powder includes TiC, Al2O3, at least one of WC, SiC, TiN, or C and/
Or B4C, wherein, C and B4C with metallic element reaction generation mainly by strengthening phase.
Further preferred scheme, the particle diameter of the enhancing phase powder is 1nm~10 μm.
It is preferred that scheme, during V-type batch mixer or low energy ball milling mixing in order to prevent oxidation, can be in batch mixing
Protective gas, such as inert gas are filled with device.
It is preferred that scheme, the powder metallurgic method include hot pressing, molding-sintering, isostatic cool pressing-sintering or high temperature insostatic pressing (HIP).
More preferably scheme, in order to reach that preferably electrode sensing is required, the relative density of composite bar (actual density with
The ratio of solid density) it is preferably up to more than 95%.
It is preferred that scheme, a diameter of 30~150mm of the composite bar.
It is preferred that 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), choose needed for particle size range powder can be used to PM technique
Composite is prepared with 3D printing technique.
The problem of there is poor fluidity in existing particulate reinforced metal-based composite powder material, impurity content is high, and it is existing
Although aerosolization technology can prepare the metal powder material of good fluidity, exist to be difficult to prepare enhancing and be mutually uniformly distributed
Metal Substrate strengthen phase composite powder defect.Present invention firstly provides use simple and mechanical mixing+powder metallurgic method shaping+nothing
Crucible induction melting Gas atomization techniques prepare the group technology of powder, successfully prepare enhancing and are mutually uniformly distributed, and mobility
It is good, the high particulate reinforced metal-based composite powder material of purity.It is first by V-type batch mixer or simple using low energy ball milling etc.
Mechanical mixture technique can realize the mixing of powder stock, and powder in high-energy ball milling mixed process can be avoided to pollute.
On the basis of this, mixed-powder is shaped and is sintered to compound using the conventional powder metallurgic method such as technology such as powder cold pressing or hot pressing
Bar, overcomes conventional melting to cause enhancing to be separated or shortcoming pockety.The present invention is further using without crucible sensing
Melting Gas atomization techniques carry out powder by atomization, by using without crucible induction melting gas atomization equipment, because it is without in
Between bag and mozzle, can be achieved high viscosity metal bath prepare powder body material, can be prevented effectively from composite granule raw material melting
During enhancing in molten matrix metal precipitation, so as 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, the advantageous effects that technical scheme is brought：
1st, particulate reinforced metal-based complex spherical powder material prepared by the present invention is spherical or subsphaeroidal for standard, with stream
Dynamic property is good, the characteristics of apparent density is excellent, and preparation process impurity introduction volume is low, can guarantee that the high-purity feature of powder body material,
Meanwhile, enhancing be mutually evenly distributed in metallic matrix, be conducive to obtain high-performance composite materials, be highly suitable for powder metallurgy and
3D printing increasing material manufacturing raw material.
2nd, 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 the poor fluidity that exists of mixed-powder, purity is low and enhancing mutually can not the technology of accuracy controlling ask
Topic.Meanwhile, using the powder for preparing of the present invention as raw material, can on conventional 3D printer forming metal based composites, improve
The universality of conventional 3D printing equipment.
3rd, without high-energy ball milling during the present invention prepares particulate reinforced metal-based complex spherical powder material, it can reduce
Impurity in mixed-powder is introduced, while using without crucible for smelting aerosolization technology, it is to avoid contact of the molten metal with crucible, is prepared
Powder purity it is higher.
4th, to metal matrix material and increasing during the present invention prepares particulate reinforced metal-based complex spherical powder material
The species and proportioning of strong particle are alternative strong, and material designability is strong.
5th, the technique of the invention for preparing particulate reinforced metal-based complex spherical powder material is simple, and equipment is ripe, can be used for
Industrial mass production.
Brief description of the drawings
【Fig. 1】The process chart of spherical metal base composite powder is prepared for the present invention.
【Fig. 2】For without crucible for smelting aerosolizing device schematic diagram.
【Fig. 3】The spherical Ti6Al4V/TiC composite powders pattern prepared for the present invention.
【Fig. 4】TiC distribution map in the spherical Ti6Al4V/TiC composite powders prepared for the present invention.
Embodiment
Below by the present invention is described further in conjunction with the embodiments.The present embodiment is served only for saying to the present invention
It is bright, it is not intended to limit to protection scope of the present invention.
Embodiment 1
For preparing titanium alloy composite powder
From the TiC powder that aerosolization Ti6Al4V powder that particle diameter is 10 μm~150 μm and particle diameter are 1.5 μm, according to
Lower mass percent carries out dispensing：95wt.% Ti6Al4V alloy powders, 5wt.% TiC.It will be weighed according to above-mentioned formula
Powder be placed in V-type batch mixer, to prevent that powder is aoxidized in mixing process, vacuumizes after mixing tank is sealed, be re-filled with
Argon gas.Batch mixing rotating speed is 100rad/min, and the time is 2h.Mixed-powder is put into a diameter of 35mm graphite hot pressing die, is
The pollution of charcoal in graphite jig is prevented, BN lubricants are coated in mould inner wall.Sintering temperature is 1100 DEG C, and pressure is 16MPa, is protected
Warm time 1h, sintering atmosphere is protected for argon gas.Composite bar one end after terminating is machined as to 70 ° of cone angle, surface
Polished with sand paper.Using without crucible induction melting aerosolizing device, argon gas is atomization gas, control charging rate for 20~
40mm/min, 3.5~8.0MPa of atomizing pressure, can be made the equally distributed composite powders of hardening constituent TiC.It is aobvious using scanning electron
Micro mirror carries out sphericity observation to powder, and powder is spherical or subsphaeroidal.
Embodiment 2
For preparing titanium-based composite powder
The B for being 400nm from the irregular pure Ti powder that particle diameter is 10 μm~60 μm and particle diameter4C powder, according to following
Mass percent carries out dispensing：98wt.% Ti powder, 2wt.% B4C.The powder weighed according to above-mentioned formula is placed in ball
Grinding jar, ratio of grinding media to material is 1:1, mill ball material used is 201 stainless steels.To prevent that powder is aoxidized in mixing process, by ball
Vacuumized after grinding jar sealing, be re-filled with argon gas.Rotational speed of ball-mill is 250rad/min, and Ball-milling Time is 4h.Mixed-powder is put into
A diameter of 50mm rubber package set, is molded in isostatic cool pressing equipment, and briquetting pressure is 250MPa.After isostatic cool pressing
Pressed compact is sintered in vacuum sintering furnace, and sintering temperature is 1400 DEG C, soaking time 2h.By the composite bar after terminating
One end is machined as 60 ° of cone angle, and sand for surface paper is polished.Using without crucible induction melting aerosolizing device, (if
Independent research, must) argon gas is atomization gas, control charging rate for 25~35mm/min, atomizing pressure 3.5~
6.0MPa, can be made the equally distributed composite powder of hardening constituent TiC and TiB.Ball is carried out to powder using SEM
Shape degree is observed, and powder is spherical or subsphaeroidal.
Embodiment 3
For preparing aluminium alloy compound powder
From the AlN powder that aerosolization AlSi10Mg powder that particle diameter is 10 μm~150 μm and particle diameter are 2.0 μm, according to
Following mass percent carries out dispensing：96wt.% AlSi10Mg alloy powders, 4wt.% AlN.It will claim according to above-mentioned formula
The powder taken is placed in ball grinder, and ratio of grinding media to material is 2:1, mill ball material used is corundum (Al2O3).To prevent powder in mixing process
End is aoxidized, and is vacuumized 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.Mixed-powder is put into a diameter of 45mm graphite hot pressing die.Sintering temperature is 610 DEG C, and pressure is 12MPa, insulation
Time 1.5h, sintering atmosphere is protected for argon gas.Composite bar one end after terminating is machined as to 120 ° of cone angle, surface
Polished with sand paper.Using without crucible induction melting aerosolizing device, nitrogen is atomization gas, control charging rate for 30~
50mm/min, 2.0~4.0MPa of atomizing pressure, can be made the equally distributed composite powders of hardening constituent AlN.It is aobvious using scanning electron
Micro mirror carries out sphericity observation to powder, and powder is spherical or subsphaeroidal.
Claims (8)
1. a kind of strengthen the preparation method of mutually equally distributed particulate reinforced metal-based complex spherical powder material, its feature exists
In：Metal dust is used after V-type batch mixer or low energy ball milling mixing with enhancing phase powder, passes through powder metallurgic method and is molded and burns
Knot prepares composite bar；The composite bar is particulate reinforced metal-based multiple using being prepared without crucible induction melting gas atomization equipment
Close spherical powder material；The charging rate without 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.
2. the preparation of the mutually equally distributed particulate reinforced metal-based complex spherical powder material of enhancing according to claim 1
Method, it is characterised in that：The metal dust is included more than one or both of iron-based, Ni-based, aluminium base, copper-based, titanium-based
Element powders or alloy powder.
3. the preparation of the mutually equally distributed particulate reinforced metal-based complex spherical powder material of enhancing according to claim 2
Method, it is characterised in that：The particle diameter of the metal dust is 1~500 μm.
4. the preparation of the mutually equally distributed particulate reinforced metal-based complex spherical powder material of enhancing according to claim 1
Method, it is characterised in that：The enhancing phase powder includes TiC, Al2O3, WC, SiC, at least one of TiN powder, or can be with
The C and/or B of basic metallic element reaction generation enhancing phase4C powder.
5. the mutually equally distributed particulate reinforced metal-based complex spherical powder of enhancing according to any one of Claims 1 to 4
The preparation method of material, it is characterised in that：The particle diameter of the enhancing phase powder is 1nm~10 μm.
6. the mutually equally distributed particulate reinforced metal-based complex spherical powder of enhancing 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
Isostatic pressed.
7. the mutually equally distributed particulate reinforced metal-based complex spherical powder of enhancing according to any one of Claims 1 to 4
The preparation method of material, it is characterised in that：Composite bar relative density of the mixed-powder after shaping and sintering is more than 95%.
8. the mutually equally distributed particulate reinforced metal-based complex spherical powder of enhancing according to any one of Claims 1 to 4
The preparation method of material, it is characterised in that：A diameter of 30~150mm of the composite bar.
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| CN108516808A (en) * | 2018-07-10 | 2018-09-11 | 哈尔滨工业大学 | The method that high-temperature fusant aeroponics prepare alumina-based nano eutectic composite micro-powder |
| CN109513943A (en) * | 2019-01-07 | 2019-03-26 | 华南理工大学 | A kind of 3D printing Al alloy powder and preparation method through nano-ceramic particle modification |
| CN109550963A (en) * | 2018-12-13 | 2019-04-02 | 华南理工大学 | A kind of sub-micron hydride particle enhancing aluminium base raw powder's production technology for 3D printing |
| CN109852830A (en) * | 2019-01-15 | 2019-06-07 | 中南大学 | A kind of superfine carbide particles reiforced metal-base composition and preparation method thereof |
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| CN110014158A (en) * | 2019-04-22 | 2019-07-16 | 西安斯瑞先进铜合金科技有限公司 | A kind of method that aerosolization prepares spherical chromium powder |
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