CN108380865A - Laser gain material manufacture 6XXX systems in-situ Al-base composition powder and preparation - Google Patents
Laser gain material manufacture 6XXX systems in-situ Al-base composition powder and preparation Download PDFInfo
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- CN108380865A CN108380865A CN201810096873.5A CN201810096873A CN108380865A CN 108380865 A CN108380865 A CN 108380865A CN 201810096873 A CN201810096873 A CN 201810096873A CN 108380865 A CN108380865 A CN 108380865A
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- 239000000843 powder Substances 0.000 title claims abstract description 73
- 239000000463 material Substances 0.000 title claims abstract description 54
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 239000000203 mixture Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 32
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910033181 TiB2 Inorganic materials 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 20
- 239000000956 alloy Substances 0.000 claims abstract description 20
- 229910020491 K2TiF6 Inorganic materials 0.000 claims abstract description 19
- 229910020261 KBF4 Inorganic materials 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000000155 melt Substances 0.000 claims abstract description 19
- 238000007670 refining Methods 0.000 claims abstract description 18
- 238000012387 aerosolization Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 7
- 239000004411 aluminium Substances 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 4
- 238000010792 warming Methods 0.000 claims description 12
- 239000006227 byproduct Substances 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 7
- 229910018125 Al-Si Inorganic materials 0.000 claims description 5
- 229910018520 Al—Si Inorganic materials 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 238000000889 atomisation Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 11
- 239000008187 granular material Substances 0.000 abstract description 9
- 238000009689 gas atomisation Methods 0.000 abstract description 6
- 239000002023 wood Substances 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 11
- 239000010936 titanium Substances 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 7
- 230000004224 protection Effects 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 238000005275 alloying Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 239000000443 aerosol Substances 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
Classifications
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- B22F1/0003—
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- 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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
-
- 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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/10—Inert gases
- B22F2201/11—Argon
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/10—Inert gases
- B22F2201/12—Helium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention provides the preparation methods that a kind of laser gain material manufactures 6XXX systems in-situ Al-base composition powder, including commercial-purity aluminium is heated, and heat up melting after being covered with high temperature covering agent;By KBF4、K2TiF6Uniformly mixing is added after drying in melt;After reaction, required intermediate alloy and technical pure Mg are sequentially added, refining agent is added in the melt and carries out refinery by de-gassing, then carries out aerosolization;To obtain the final product.This method is prepared for TiB in situ using melt-growth in situ and High Temperature Gas atomization method2Micro-nano granules enhance 6XXX composite materials, by preparing TiB2Particle reinforced aluminium-based composite wood powder, TiB2Particle even dispersion is distributed in aluminum substrate.Aluminum matrix composite powder prepared by this method has good laser absorption rate, is suitable for laser gain material manufacturing technology.
Description
Technical field
The invention belongs to technical field of material, and 6XXX systems aluminum-base composite is manufactured more particularly, to a kind of laser gain material
Material powder and preparation method.
Background technology
With the development of modern science and technology, the requirement in practical application to material property and technology of preparing becomes more severe
It carves.Contour leading-edge field especially is manufactured in aerospace, weapons, structural material is requiring have the same of high-strength high-plasticity
When, should also have high specific stiffness and specific modulus.The high-end equipment field such as large aircraft is to high-performance, high reliability, economy
With the pursuit of environmental protection, cause the demand to large-scale, accurate, the complicated high tough alloy components of integral light more and more urgent.Laser
Increases material manufacturing technology can solve to take into account the technical barrier that complicated shape and high-performance metal component quickly manufacture, and become solution
The certainly effective way of aerospace manufacturing field key technology difficulty.
However commercialized metal powder is mainly pre-alloying powder prepared by atomization or rotary electrode method at present, by
It is formed on the limitation of the key technical index such as laser absorption rate, alloy powder type available at present is limited.Especially in aluminium
Alloy by Laser material increasing field, since aluminium alloy laser absorption rate is relatively low, only the alloy powder of Al-Si systems is relatively suitable at present
It shares and is manufactured in laser gain material, significantly limit the laser gain material manufacturing technology development of alumina-base material.Currently, utilizing such quotient
Industry powder has prepared the parts of higher dimensional precision, and in aerospace, and the fields such as medical treatment obtain some applications.
Such as Boeing companies of the U.S. start LCD large titanium alloy parts being applied to F-18 and F-22 fighter planes since two thousand,
And the United States Patent (USP) in 2015 having applied for airplane parts increasing material manufacturing system.European AirBus companies start since two thousand six
Undercarriage LCD technology is attempted, and is combined topology optimization design with SLM technologies, realizes titanium alloy engine nacelle
The optimization of hinge manufactures.The forefront in SLM technical research and application is then walked by GE companies of the U.S., and SLM technologies is used to manufacture
T25 engine sensor shells have been used for GE90-94B aero-engines, and are answered by the approval aviation of Federal Aviation management board
With.But the part prepared is also easy to produce the defects of crackle and hole of higher residual stress and micron level, and then lead to material
Expect that fatigue strength, plasticity and toughness reduce.Thus part production yield rate is low, reliability is insufficient and cost remains high.Therefore
Traditional business alloy powder cannot fully meet the manufacture of high-performance components.
Invention content
The present invention is limited for above-mentioned material system and Improvement requirement, it is proposed that a kind of laser gain material manufacture 6XXX systems original
Position aluminum matrix composite powder and preparation method, high laser absorption rate can be provided simultaneously with by having prepared, the high aluminium of particle spherical shape rate
Based composites powder, and technological operation is simple and practicable, low-cost high-efficiency, is appropriate for producing in batches.
The purpose of the present invention is what is be achieved through the following technical solutions:
The present invention provides the preparation method that a kind of laser gain material manufactures 6XXX systems in-situ Al-base composition powder, packets
Include following steps:
A1, commercial-purity aluminium is heated, heat up melting after being covered with high temperature covering agent;
A2, by KBF4、K2TiF6Uniformly mixing is added after drying in the melt that step A1 is obtained, mechanical agitation;
A3, after step A2 reaction, take out byproduct of reaction, sequentially add required intermediate alloy and technical pure Mg,
Refining agent is added in the melt and carries out refinery by de-gassing, controlled at 700~800 DEG C of 10~20min of standing, then 700~
800 DEG C of progress aerosolizations;6XXX systems in-situ Al-base composition powder is manufactured up to the laser gain material.
Preferably, in step A1, the high temperature covering agent is JZF-03 type high temperature covering agents.
Preferably, described to be warming up to 650~950 DEG C of meltings in step A1.
Preferably, in step A2, the KBF4、K2TiF6Mass ratio be 1:0.5~1:2.
Preferably, in step A2, the reaction time is 5-60min.
Preferably, in step A3, the refining agent is the harmless aluminum refining agent of JZJ types.
Preferably, in step A3, the aerosolization the specific steps are:Solution is warming up to 750~1200 DEG C, uses Ar
And/or be atomized under He gas shields, 0.5~10MPa of atomization air pressure, it is atomized 0.5~5mm of nozzle diameter of use.Using
The aerosolization parameter area can make powder spherical shape rate, the recovery rate highest of acquisition.If in the range, can not cause
Spherical rate, recovery rate decline.
The present invention also provides a kind of laser gain material manufacture prepared according to preceding method is compound with 6XXX systems in-situ Al-base
Material powder, the group of the aluminum matrix composite become Al-Si (1%~15%)-Mg (1%~8%)-Zr (0.05%~
3%)-Sc (0%~3%)-Mn (0%~2%)-Ti (0%~1%).
Preferably, the group of the aluminum matrix composite becomes Al-Si (1%~15%)-Mg (1%~8%)-Zr
(0.05%~3%)-Sc (0.05%~3%)-Mn (0.05%~2%)-Ti (0.01%~1%).The present invention adds simultaneously
Tetra- kinds of trace elements of Zr, Sc, Mn, Ti can make the mechanical property for the sample that the laser gain material of acquisition subsequently manufactures best.
The micro- Mn that the present invention adds is a kind of common to carry high performance alloying element;Present invention addition is micro
Sc, Ti element can significantly crystal grain thinning, and adding micro Zr elements simultaneously can keep except this advantage, improve material
The stability of material in the high temperature environment.In conclusion addition Zr, Sc, Mn, Ti can improve post laser increasing material manufacturing sample
Mechanical property.
Preferably, the median particle diameter of the 6XXX systems in-situ Al-base composition powder is 2~175 μm, and spherical rate is more than
90%;In the 6XXX systems in-situ Al-base composition powder, including the nanoscale TiB that mass fraction is 0.5%~10%2
Grain, the nanoscale TiB2In the distribution of particle even dispersion and aluminum substrate, the TiB2Particle size is 5~2200nm.It is described
TiB2The mass fraction of particle can cause density of material to rise beyond above range, and toughness significantly reduces, or even can not be prepared into
To spherical powder.
Preferably, the grain structure of the 7XXX systems in-situ Al-base composition powder is equiax crystal, and crystallite dimension is
0.1~5.5 μm.
Compared with the prior art, the substantive distinguishing features and significant progress that the present invention has are:
1) present invention has been effectively combined the advantage that melt-growth in situ prepares micro-nano particle reinforced.
The aluminum matrix composite powder of micro-nano granules enhancing, powder particle median particle diameter are prepared by the method for melt-growth in situ
Controllable, spherical rate > 90%, recovery rate >=60% at 2~175 μm;The micro-nano TiB of in-situ authigenic in dispersion composite material2
Grain, TiB2Particle size distribution is between 5-2200nm, and while greatly improving the strength of materials, the powder that effectively improves swashs
Absorptivity (>40%) the material application range of alumina-base material laser gain material manufacture, is substantially extended.
2) laser gain material manufacture is carried out using the 6XXX composite powders, it is made relative to traditional al-si system powder
Standby strength of materials plasticity is higher, due to nanometer TiB2The humidification of particle and the effect for inhibiting recrystallization growth can be obtained
Uniformly tiny equiax crystal, grain size distribution is in 0.1-5.5 μm.Due in microstructure of composite even dispersion be distributed it is micro-
Nanometer TiB2The presence of particle and tiny equiax crystal, laser gain material prepared by the method for the present invention manufacture aluminum matrix composite component
Can have high intensity and high-ductility simultaneously.
Description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 aerosolizing device schematic diagrames of the present invention;
Fig. 2 is the SEM photograph of aluminum matrix composite powder prepared by embodiment 1;Wherein, figure (a) is powder entirety photo,
It is single powder section macrograph to scheme (b).
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, several changes and improvements can also be made.These belong to the present invention
Protection domain.
Following embodiment provides a kind of preparation side of laser gain material manufacture 6XXX systems in-situ Al-base composition powder
Method includes the following steps:
A1, commercial-purity aluminium is heated, heat up melting after being covered with high temperature covering agent;
A2, by KBF4、K2TiF6Uniformly mixing is added after drying in the melt that step A1 is obtained, mechanical agitation;
A3, after step A2 reaction, take out byproduct of reaction, sequentially add required intermediate alloy and technical pure Mg,
Refining agent is added in the melt and carries out refinery by de-gassing, controlled at 700~800 DEG C of 10~20min of standing, then 700~
800 DEG C of progress aerosolizations;6XXX systems in-situ Al-base composition powder is manufactured up to the laser gain material.
In step A1, the high temperature covering agent is JZF-03 type high temperature covering agents.
It is described to be warming up to 650~950 DEG C of meltings in step A1.
In step A2, the KBF4、K2TiF6Mass ratio be 1:0.5~1:2.
In step A2, the reaction time is 5-60min.
In step A3, the refining agent is the harmless aluminum refining agent of JZJ types.
In step A3, the aerosolization the specific steps are:Solution is warming up to 750~1200 DEG C, uses Ar and/or He gas
It is atomized under body protection, 0.5~10MPa of atomization air pressure is atomized 0.5~5mm of nozzle diameter of use.Using the aerosol
Change parameter area, powder spherical shape rate, the recovery rate highest of acquisition can be made.If spherical rate in the range, can not caused, received
Rate declines.
Following embodiment additionally provides a kind of laser gain material manufacture 6XXX systems in-situ Al-base prepared according to preceding method
The group of composite powder, the aluminum matrix composite becomes Al-Si (1%~15%)-Mg (1%~8%)-Zr (0.05%
~3%)-Sc (0%~3%)-Mn (0%~2%)-Ti (0%~1%).
The micro- Mn that the present invention adds is a kind of common to carry high performance alloying element;Present invention addition is micro
Sc, Ti element can significantly crystal grain thinning, and adding micro Zr elements simultaneously can keep except this advantage, improve material
The stability of material in the high temperature environment.In conclusion addition Zr, Sc, Mn, Ti can improve post laser increasing material manufacturing sample
Mechanical property.The present invention adds tetra- kinds of trace elements of Zr, Sc, Mn, Ti, the examination that the laser gain material of acquisition can be made subsequently to manufacture simultaneously
The mechanical property of sample is best.
The median particle diameter of the 6XXX systems in-situ Al-base composition powder is 2~175 μm, and spherical rate is more than 90%;Institute
It states in 6XXX systems in-situ Al-base composition powder, including the nanoscale TiB that mass fraction is 0.5%~10%2Particle, it is described
Nanoscale TiB2In the distribution of particle even dispersion and aluminum substrate, the TiB2Particle size is 5~2200nm.The TiB2Particle
Mass fraction density of material can be caused to rise beyond above range, toughness significantly reduces, or even spherical powder can not be prepared
End.
The grain structure of the 7XXX systems in-situ Al-base composition powder is equiax crystal, and crystallite dimension is 0.1~5.5
μm。
Embodiment 1
Experiment is with high-purity Al, technical pure Mg, Al-12Si, Al-12Zr intermediate alloy, KBF4And K2TiF6Match for raw material
In-situ authigenic 5wt.%TiB is made2REINFORCED Al -6.7Si-2.2Mg-0.1Zr composite materials.First high-purity Al is put into crucible and is melted
Change and be warming up to 780 DEG C, with the covering of JZF-03 type high temperature covering agents;By KBF4、K2TiF6In mass ratio 1:2 after evenly mixing, dries
In the melt being added after dry;It waits for after reaction, taking out byproduct of reaction, sequentially adding Al-12Si, Al-12Zr intermediate alloy
And technical pure Mg, the harmless aluminum refining agent of JZJ types is added in the melt and carries out refinery by de-gassing, is stood at 800 DEG C
15min, then gas-atomized powder.Its aerosolization (aerosolizing device is as shown in Figure 1) technique is:870 DEG C of solution temperature, uses He
Protect simultaneously aerosolization, air pressure 2.22MPa, nozzle diameter 2.16mm.The SEM photograph of gained composite powder is as shown in Fig. 2, institute
34.4 μm of powder average diameter obtained, spherical rate > 90%, recovery rate >=60%, TiB2Granule content 5wt.%, composite wood
1.8 μm of feed powder end average grain size, laser absorption rate 47%.
Embodiment 2
Experiment is with high-purity Al, technical pure Mg, Al-12Si, Al-12Zr intermediate alloy, KBF4And K2TiF6Match for raw material
In-situ authigenic 5wt.%TiB is made2REINFORCED Al -6.6Si-2.2Mg-0.09Zr composite materials.First high-purity Al is put into crucible
It melts and is warming up to 780 DEG C, with the covering of JZF-03 type high temperature covering agents;By KBF4、K2TiF6In mass ratio 1:2 after evenly mixing,
It is added in melt after drying;It waits for after reaction, taking out byproduct of reaction, sequentially adding Al-12Si, Al-12Zr intermediate alloy
And technical pure Mg, the harmless aluminum refining agent of JZJ types is added in the melt and carries out refinery by de-gassing, is stood at 750 DEG C
20min, then gas-atomized powder.Its gas atomization is:900 DEG C of solution temperature uses He protections and aerosolization, air pressure
3.30MPa, nozzle diameter 1.5mm.18 μm of obtained powder average diameter, spherical rate > 90%, recovery rate >=60%, TiB2
Granule content 5wt.%, 1.0 μm of composite powder average grain size, laser absorption rate 45%.
Embodiment 3
Experiment is with high-purity Al, technical pure Mg, Al-12Si, Al-12Zr intermediate alloy, KBF4And K2TiF6Match for raw material
In-situ authigenic 5wt.%TiB is made2REINFORCED Al -6.6Si-2.2Mg-0.09Zr composite materials.First high-purity Al is put into crucible
It melts and is warming up to 780 DEG C, with the covering of JZF-03 type high temperature covering agents;By KBF4、K2TiF6In mass ratio 1:2 after evenly mixing,
It is added in melt after drying;It waits for after reaction, taking out byproduct of reaction, sequentially adding Al-12Si, Al-12Zr intermediate alloy
And technical pure Mg, the harmless aluminum refining agent of JZJ types is added in the melt and carries out refinery by de-gassing, is stood at 750 DEG C
15min, then gas-atomized powder.Its gas atomization is:900 DEG C of solution temperature uses Ar protections and aerosolization, air pressure
1.20MPa, nozzle diameter 2.16mm.45 μm of obtained powder average diameter, spherical rate > 90%, recovery rate >=60%,
TiB2Granule content 5wt.%, 2.2 μm of composite powder average grain size, laser absorption rate 45%.
Embodiment 4
Experiment is with high-purity Al, technical pure Mg, Al-12Si, Al-10Mn, Al-12Zr intermediate alloy, KBF4And K2TiF6For
Raw material have prepared in-situ authigenic 10wt.%TiB2REINFORCED Al -6.6Si-2.2Mg-0.7Mn-0.09Zr composite materials.It first will be high
Pure Al, which is put into crucible, melts and is warming up to 780 DEG C, is covered with JZF-03 type high temperature covering agents;By KBF4、K2TiF6In mass ratio
1:2 after evenly mixing, is added in melt after drying;Wait for after reaction, take out byproduct of reaction, sequentially add Al-12Si,
Al-10Mn, Al-12Zr intermediate alloy and technical pure Mg are added the harmless aluminum refining agent of JZJ types and carry out degasification in the melt
Refining, stands 15min, then gas-atomized powder at 780 DEG C.Its gas atomization is:900 DEG C of solution temperature, is protected using Ar
Protect simultaneously aerosolization, air pressure 5.10MPa, nozzle diameter 2.16mm.23 μm of obtained powder average diameter, spherical rate > 90%,
Recovery rate >=60%, TiB2Granule content 10wt.%, 1.5 μm of composite powder average grain size, laser absorption rate
67%.
Embodiment 5
Experiment is with high-purity Al, technical pure Mg, Al-12Si, Al-10Mn, Al-12Zr intermediate alloy, KBF4And K2TiF6For
Raw material have prepared in-situ authigenic 8wt.%TiB2REINFORCED Al -6.6Si-2.2Mg-0.7Mn-0.09Zr composite materials.It first will be high
Pure Al, which is put into crucible, melts and is warming up to 780 DEG C, is covered with JZF-03 type high temperature covering agents;By KBF4、K2TiF6In mass ratio
1:2 after evenly mixing, is added in melt after drying;Wait for after reaction, take out byproduct of reaction, sequentially add Al-12Si,
Al-10Mn, Al-12Zr intermediate alloy and technical pure Mg are added the harmless aluminum refining agent of JZJ types and carry out degasification in the melt
Refining, stands 15min, then gas-atomized powder at 750 DEG C.Its gas atomization is:900 DEG C of solution temperature, uses 50%
Ar and 50%He mixing gas shielded and aerosolization, air pressure 3.07MPa, nozzle diameter 1.7mm.Obtained powder average diameter 22
μm, spherical rate > 90%, recovery rate >=60%, TiB2Granule content 8wt.%, 1.3 μ of composite powder average grain size
M, laser absorption rate 57%.
Embodiment 6
Experiment with high-purity Al, technical pure Mg, Al-12Si, Al-10Mn, Al-12Zr, Al-2Sc, Al-10Ti intermediate alloy,
KBF4And K2TiF6In-situ authigenic 5wt.%TiB has been prepared for raw material2REINFORCED Al -6.6Si-2.2Mg-0.7Mn-0.1Zr-
0.1Sc-0.01Ti composite materials.First high-purity Al is put into crucible and melts and be warming up to 780 DEG C, is covered with JZF-03 type high temperature
Agent covers;By KBF4, K2TiF6 in mass ratio 1:2 after evenly mixing, is added in melt after drying;It waits for after reaction, taking out
Byproduct of reaction sequentially adds Al-12Si, Al-12Zr, Al-2Sc, Al-10Mn, Al-10Ti intermediate alloy and technical pure
Mg is added the harmless aluminum refining agent of JZJ types and carries out refinery by de-gassing, 15min stood at 750 DEG C, then aerosol in the melt
Change powder processed.Its gas atomization is:900 DEG C of solution temperature uses Ar protections and aerosolization, air pressure 3.07MPa, nozzle diameter
2.16mm.24 μm of obtained powder average diameter, spherical rate > 90%, recovery rate >=60%, TiB2 granule content 5wt.%,
1.2 μm of composite powder average grain size, laser absorption rate 45%.
Embodiment 7
The present embodiment and the experimental procedure of embodiment 6 are essentially identical, the difference is that only:This comparative example has prepared original position
Spontaneous 0.5wt.%TiB2REINFORCED Al -6.6Si-2.2Mg-0.7Mn-0.1Zr-0.1Sc-0.01Ti composite materials.Obtained
38 μm of powder average diameter, spherical rate > 90%, recovery rate >=60%, TiB2Granule content 0.5wt.%, composite powder
3.4 μm of average grain size, laser absorption rate 41%.
It is prepared for subsequent sample using laser gain material made from 1-7 of the embodiment of the present invention, obtains extraordinary power
Learn performance.The mechanical property of especially embodiment 6 and 7 is best.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or change within the scope of the claims, this not shadow
Ring the substantive content of the present invention.In the absence of conflict, the feature in embodiments herein and embodiment can arbitrary phase
Mutually combination.
Claims (10)
1. a kind of preparation method of laser gain material manufacture 6XXX systems in-situ Al-base composition powder, which is characterized in that including
Following steps:
A1, commercial-purity aluminium is heated, heat up melting after being covered with high temperature covering agent;
A2, by KBF4、K2TiF6Uniformly mixing is added after drying in the melt that step A1 is obtained, and mechanical agitation is reacted;
A3, after step A2 reaction, pure Mg is added refining agent and carries out refinery by de-gassing in the melt, controlled at 700~take out
Byproduct of reaction sequentially adds 800 DEG C of 10~20min of standing of required intermediate alloy and industry, then at 700~800 DEG C
Carry out aerosolization;6XXX systems in-situ Al-base composition powder is manufactured up to the laser gain material.
2. the preparation method of laser gain material manufacture 6XXX systems in-situ Al-base composition powder according to claim 1,
It is characterized in that, in step A1, the high temperature covering agent is JZF-03 type high temperature covering agents.
3. the preparation method of laser gain material manufacture 6XXX systems in-situ Al-base composition powder according to claim 1,
It is characterized in that, in step A1, it is described to be warming up to 650~950 DEG C of meltings.
4. the preparation method of laser gain material manufacture 6XXX systems in-situ Al-base composition powder according to claim 1,
It is characterized in that, in step A2, the KBF4、K2TiF6Mass ratio be 1:0.5~1:2.
5. the preparation method of laser gain material manufacture 6XXX systems in-situ Al-base composition powder according to claim 1,
It is characterized in that, in step A2, the reaction time is 5-60min.
6. the preparation method of laser gain material manufacture 6XXX systems in-situ Al-base composition powder according to claim 1,
It is characterized in that, in step A3, the refining agent is the harmless aluminum refining agent of JZJ types.
7. the preparation method of laser gain material manufacture 6XXX systems in-situ Al-base composition powder according to claim 1,
It is characterized in that, in step A3, the aerosolization the specific steps are:Solution is warming up to 750~1200 DEG C, using Ar and/or
It is atomized under He gas shields, 0.5~10MPa of atomization air pressure, is atomized 0.5~5mm of nozzle diameter of use.
8. laser gain material prepared by a kind of method according to claim 1 manufactures 6XXX systems in-situ Al-base composition powder
End, which is characterized in that the group of the aluminum matrix composite becomes Al-Si (1%~15%)-Mg (1%~8%)-Zr (0.05%
~3%)-Sc (0%~3%)-Mn (0%~2%)-Ti (0%~1%).
9. the laser gain material that according to claim 8 prepared by method manufactures 6XXX systems in-situ Al-base composition powder,
It is characterized in that, the median particle diameter of the 6XXX systems in-situ Al-base composition powder is 2~175 μm, and spherical rate is more than 90%;Institute
It states in 6XXX systems in-situ Al-base composition powder, including the nanoscale TiB that mass fraction is 0.5%~10%2Particle, it is described
Nanoscale TiB2In the distribution of particle even dispersion and aluminum substrate, the TiB2Particle size is 5~2200nm.
10. the laser gain material that according to claim 9 prepared by method manufactures 6XXX systems in-situ Al-base composition powder,
It being characterized in that, the grain structure of the 6XXX systems in-situ Al-base composition powder is equiax crystal, crystallite dimension is 0.1~
5.5μm。
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