CN110512111A - The preparation method of in-situ Al-base composition - Google Patents
The preparation method of in-situ Al-base composition Download PDFInfo
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- CN110512111A CN110512111A CN201910258317.8A CN201910258317A CN110512111A CN 110512111 A CN110512111 A CN 110512111A CN 201910258317 A CN201910258317 A CN 201910258317A CN 110512111 A CN110512111 A CN 110512111A
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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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
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- 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
- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
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- 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
- C22C21/12—Alloys based on aluminium with copper as the next major constituent
- C22C21/16—Alloys based on aluminium with copper as the next major constituent with magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
Abstract
The invention discloses a kind of preparation methods of in-situ Al-base composition comprising following steps: high temperature covering agent being added in fine aluminium, carries out melting, obtains melt;KBF is added into the melt4And KTiF6, mix and reacted;After removing by-product, sequentially add aluminum bronze intermediate alloy, aluminium zirconium hardener, scandium bearing master alloy, aluminium manganese intermediate alloy, aluminium titanium intermediate alloy and pure magnesium, and harmless aluminum refining agent is added, refinery by de-gassing and aerosolization are successively carried out at 700~850 DEG C, obtain in-situ self-generated TiB2The Al-Cu-Mg composite powder of particle enhancing.The present invention, which has prepared, can be provided simultaneously with high laser absorption rate, the high aluminum matrix composite powder of particle spherical shape rate, and technological operation is simple and easy, low-cost high-efficiency, is appropriate for producing in batches.
Description
Technical field
The present invention relates to a kind of preparation methods of in-situ Al-base composition, belong to field of material technology.
Background technique
In recent years, the rapid development of the high-end equipment field such as weapons manufacture, aerospace proposes the performance of material and preparation
Gone out increasingly harsher requirement: structural material other than having high specific stiffness and specific modulus, must have high-ductility and
It is high-intensitive.Currently, the equipment manufacture industries such as large aircraft are to the tough alloy building of large-scale, accurate, complicated high-strength light
Demand is more more and more urgent, to meet its needs to high-performance, high reliability and high economy and high-environmental.Laser gain material
Manufacturing technology can cope with the key technology difficulty of the high-end manufacturing field such as above aerospace very well, obtain industry increasingly
More favors.
The method for preparing pre-alloying powder at present is mainly atomization and rotary electrode method, although they have been realized in
Commercialization, but it is limited by the limitation of the key technical index such as laser absorption rate, currently available alloy powder type is limited.It is special
It is not, in view of the lower laser absorption rate of aluminium alloy, to be suitable for laser gain material at present in aluminium alloy laser gain material manufacturing field and manufacture
Al alloy powder be only limitted to Al-Si system, seriously constrain alumina-base material in the application of laser gain material manufacturing field.Currently,
Has higher dimensional precision using the components that such commercialization powder prepares, and in fields such as aerospace, medical treatment
Obtain some applications.Such as GE aero-engine business department, the U.S. realizes the light weight of its components using laser gain material manufacture
Metaplasia produces, and optimizes and exempt from the monoblock type manufacture of assembling by product design to promote the performance of aviation components.It is manufactured
Sensor outer housing obtained the certification in Federal Aviation portion, it is installed in more than 400 GE90-94B aero-engines
In.The responsible person of GE aviation GE90/GE9X once indicated, researches and develops such a components using classical production process such as castings and needs
Several years, and the use of new technology then allows product development cycle to shorten year.But the part of preparation is also easy to produce
The defects of crackle and hole of higher residual stress and micron level, so that the fatigue strength of material, plasticity and toughness are reduced,
Lead to that part production yield rate is low, reliability is insufficient and cost remains high.Therefore traditional business alloy powder cannot be complete
The manufacture of full up foot high-performance components.
Summary of the invention
The present invention is limited for above-mentioned material system and Improvement requirement, proposes a kind of laser gain material manufacture 2XXX system 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 easy, low-cost high-efficiency, is appropriate for producing in batches.
The present invention is achieved by the following technical solutions:
The present invention provides a kind of preparation methods of in-situ Al-base composition comprising following steps:
High temperature covering agent is added in fine aluminium, carries out melting, obtains melt;
KBF is added into the melt4And KTiF6, mix and reacted;
After removing by-product, sequentially add aluminum bronze intermediate alloy, aluminium zirconium hardener, scandium bearing master alloy, among aluminium manganese
Alloy, aluminium titanium intermediate alloy and pure magnesium, and harmless aluminum refining agent is added, refinery by de-gassing is successively carried out at 700~850 DEG C
And aerosolization, obtain in-situ self-generated TiB2The Al-Cu-Mg composite material of particle enhancing;
By the in-situ self-generated TiB2The Al-Cu-Mg composite material of particle enhancing carries out at the homogenization heat of alloying element
Reason.
Preferably, the temperature of the melt is 650~950 DEG C.
Preferably, the KBF4、K2TiF6Mass ratio be 1:(0.5~1:2).
Preferably, the high temperature covering agent is JZF-03 type high temperature covering agent.
Preferably, the aluminum bronze intermediate alloy, aluminium zirconium hardener, scandium bearing master alloy, aluminium manganese intermediate alloy,
The additional amount of aluminium titanium intermediate alloy and pure zinc with the metering of element in in-situ Al-base composition compare for Al-Cu (0.1%~
10%)-Mg (1%~8%)-Zr (0.05%~3%)-Sc (0.05%~3%)-Mn (0.05%~2%)-Ti (0.01%
~1%) it calculates.
Preferably, the harmless aluminum refining agent is JZJ type refining agent.
Preferably, the condition of the aerosolization are as follows: 800~1200 DEG C of melt temperature, protection gas be Ar and/or
He, air pressure are 1.5~9.5MPa, and nozzle diameter is 0.5~3mm.
Preferably, the temperature of the homogenization heat treatment is 420~580 DEG C, and the time is 6~72h.
A kind of preparation method of in-situ Al-base composition as the aforementioned manufactures 2XXX system in-situ Al-base in laser gain material
Purposes in composite material.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, in-situ self-generated TiB prepared by the present invention2The powder particle intermediate value grain of the Al-Cu-Mg composite material of particle enhancing
Diameter is controllable in 4~185 μm, and grain size distribution is in 0.5~4 μm, spherical rate > 95%, recovery rate >=80%, nanoscale
TiB2Particle even dispersion is distributed in aluminum substrate, mass fraction 0.5~10%, TiB2Particle size distribution is in 7~1500nm
Between;
2, the present invention has been effectively combined the advantage that melt-growth in situ prepares micro-nano particle reinforced.
The aluminum matrix composite powder that micro-nano granules enhancing is prepared by the method for melt-growth in situ, in dispersion composite material
The micro-nano TiB of in-situ authigenic2Particle, while greatly improving the strength of materials, the laser absorption rate (> of the powder effectively improved
28%) the material application range of alumina-base material laser gain material manufacture, is substantially extended;
3, laser gain material manufacture is carried out using the 2XXX composite powder, 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, due to the micro-nano TiB that even dispersion is distributed in microstructure of composite2Particle and tiny equiax crystal
Presence, the laser gain material manufacture aluminum matrix composite component of the method for the present invention preparation can have high-intensitive and high-ductility simultaneously.
Detailed description of the invention
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 is the SEM photograph for the aluminum matrix composite powder that in the present invention prepared by embodiment 1;Wherein, figure (a) is powder
Whole photo, figure (b) are single powder section macrograph.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.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, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
Experiment is with high-purity Al, technical pure Mg, Al-50Cu intermediate alloy, KBF4And K2TiF6Original position has been prepared for raw material
Spontaneous 5wt.%TiB2REINFORCED Al -2.2Mg-2.2Cu composite material.First high-purity Al is put into crucible and melts and is warming up to 790
DEG C, it is covered with JZF-03 type high temperature covering agent;By KBF4、K2TiF6After evenly mixing, melt is added in 1:2 in mass ratio after drying
In;To after reaction, take out byproduct of reaction, sequentially add Al-50Cu intermediate alloy and technical pure Mg, in the melt plus
Enter the harmless aluminum refining agent of JZJ type and carry out refinery by de-gassing, 15min is stood at 750 DEG C, then gas-atomized powder.Aerosolization
The technique of device are as follows: 850 DEG C of solution temperature, use He protection and aerosolization, air pressure 2.67MPa, nozzle diameter 2.16mm.It is made
Powder morphology and heterogeneous microstructure as shown in Figure 1, according to measurement and statistical analysis, it is 30.4 μm of powder average diameter, spherical
Rate > 95%, recovery rate >=58%, TiB2Granule content 5wt.%, 2.6 μm of composite powder average grain size, laser is inhaled
Yield 50%.
Embodiment 2
Experiment is with high-purity Al, technical pure Mg, Al-50Cu, Al-12Zr intermediate alloy, KBF4And K2TiF6Match for raw material
In-situ authigenic 5wt.%TiB is made2REINFORCED Al -2.2Mg-2.2Cu-0.1Zr composite material.First high-purity Al is put into crucible and is melted
Change and be warming up to 790 DEG C, with the covering of JZF-03 type high temperature covering agent;By KBF4、K2TiF61:2 in mass ratio after evenly mixing, dries
It is added in melt after dry;To after reaction, take out byproduct of reaction, sequentially add Al-50Cu, Al-12Zr intermediate alloy with
And technical pure Mg, the harmless aluminum refining agent of JZJ type is added in the melt and carries out refinery by de-gassing, stands 15min at 750 DEG C,
Then gas-atomized powder.Its gas atomization are as follows: 900 DEG C of solution temperature, use He protection and aerosolization, air pressure 3.10MPa, spray
Outspoken diameter 1.5mm.18 μm of obtained powder average diameter, spherical rate > 90%, recovery rate >=60%, TiB2Granule content
5wt.%, 1.5 μm of composite powder average grain size, laser absorption rate 50%.
Embodiment 3
Experiment is with high-purity Al, technical pure Mg, Al-50Cu, Al-12Zr intermediate alloy, KBF4And K2TiF6Match for raw material
In-situ authigenic 5wt.%TiB is made2REINFORCED Al -2.2Mg-2.2Cu-0.1Zr composite material.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 agent;By KBF4、K2TiF61:2 in mass ratio after evenly mixing, dries
It is added in melt after dry;To after reaction, take out byproduct of reaction, sequentially add Al-50Cu, Al-12Zr intermediate alloy with
And technical pure Mg, the harmless aluminum refining agent of JZJ type is added in the melt and carries out refinery by de-gassing, stands 20min at 750 DEG C,
Then gas-atomized powder.Its gas atomization are as follows: 920 DEG C of solution temperature, use Ar protection and aerosolization, air pressure 1.10MPa, spray
Outspoken diameter 2.16mm.40 μm of obtained powder average diameter, spherical rate > 88%, recovery rate >=60%, TiB2Granule content
5wt.%, 2.6 μm of composite powder average grain size, laser absorption rate 45%.
Embodiment 4
Experiment is with high-purity Al, technical pure Mg, Al-50Cu, Al-10Mn, Al-12Zr intermediate alloy, KBF4And K2TiF6For
Raw material have prepared in-situ authigenic 5wt.%TiB2REINFORCED Al -2.2Mg-2.2Cu-0.05Mn-0.1Zr composite material.It first will be high
Pure Al, which is put into crucible, melts and is warming up to 790 DEG C, is covered with JZF-03 type high temperature covering agent;By KBF4、K2TiF6In mass ratio
1:2 after evenly mixing, is added in melt after drying;To after reaction, take out byproduct of reaction, sequentially add Al-50Cu,
The harmless aluminum refining agent of JZJ type is added in the melt and carries out degasification by Al-10Mn, Al-12Zr intermediate alloy and technical pure Mg
Refining, stands 15min, then gas-atomized powder at 750 DEG C.Its gas atomization are as follows: 900 DEG C of solution temperature, use 50%
Ar and 50%He mixing gas shielded and aerosolization, air pressure 3.08MPa, nozzle diameter 1.7mm.Obtained powder average diameter 22
μm, spherical rate > 90%, recovery rate >=60%, TiB2Granule content 5wt.%, 1.5 μ of composite powder average grain size
M, laser absorption rate 50%.
Embodiment 5
Experiment is with high-purity Al, technical pure Mg, Al-50Cu, Al-10Mn, Al-12Zr intermediate alloy, KBF4And K2TiF6For
Raw material have prepared in-situ authigenic 8wt.%TiB2REINFORCED Al -2.2Mg-2.2Cu-0.05Mn-0.1Zr composite material.It first will be high
Pure Al, which is put into crucible, melts and is warming up to 800 DEG C, is covered with JZF-03 type high temperature covering agent;By KBF4、K2TiF6In mass ratio
1:2 after evenly mixing, is added in melt after drying;To after reaction, take out byproduct of reaction, sequentially add Al-50Cu,
The harmless aluminum refining agent of JZJ type is added in the melt and carries out degasification by Al-10Mn, Al-12Zr intermediate alloy and technical pure Mg
Refining, stands 15min, then gas-atomized powder at 750 DEG C.Its gas atomization are as follows: 900 DEG C of solution temperature, use 50%
Ar and 50%He mixing gas shielded and aerosolization, air pressure 3.08MPa, nozzle diameter 1.7mm.Obtained powder average diameter 22
μm, spherical rate > 90%, recovery rate >=60%, TiB2Granule content 8wt.%, 1.2 μ of composite powder average grain size
M, laser absorption rate 60%.
Embodiment 6
Experiment is with high-purity Al, technical pure Mg, Al-50Cu, Al-10Mn, Al-12Zr intermediate alloy, KBF4And K2TiF6For
Raw material have prepared in-situ authigenic 10wt.%TiB2REINFORCED Al -2.2Mg-2.2Cu-0.05Mn-0.1Zr composite material.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 agent;By KBF4、K2TiF6In mass ratio
1:2 after evenly mixing, is added in melt after drying;To after reaction, take out byproduct of reaction, sequentially add Al-50Cu,
The harmless aluminum refining agent of JZJ type is added in the melt and carries out degasification by Al-10Mn, Al-12Zr intermediate alloy and technical pure Mg
Refining, stands 15min, then gas-atomized powder at 780 DEG C.Its gas atomization are as follows: 890 DEG C of solution temperature, protected using Ar
Protect simultaneously aerosolization, air pressure 5.15MPa, nozzle diameter 2.16mm.28 μm of obtained powder average diameter, spherical rate > 90%,
Recovery rate >=65%, TiB2Granule content 10wt.%, 1.8 μm of composite powder average grain size, laser absorption rate
67%.
Embodiment 7
Experiment with high-purity Al, technical pure Mg, Al-50Cu, Al-10Mn, Al-12Zr, Al-2Sc, Al-10Ti intermediate alloy,
KBF4And K2TiF6In-situ authigenic 5wt.%TiB has been prepared for raw material2REINFORCED Al -2.2Mg-2.2Cu-0.05Mn-0.1Zr-
0.1Sc-0.01Ti composite material.First high-purity Al is put into crucible and melts and be warming up to 790 DEG C, is covered with JZF-03 type high temperature
Agent covering;By KBF4、K2TiF61:2 in mass ratio after evenly mixing, is added in melt after drying;It is anti-to after reaction, take out
By-product is answered, Al-50Cu, Al-12Zr, Al-2Sc, Al-10Mn, Al-10Ti intermediate alloy and technical pure Mg are sequentially added,
The harmless aluminum refining agent of JZJ type is added in the melt and carries out refinery by de-gassing, 15min is stood at 750 DEG C, then aerosolization system
Powder.Its gas atomization are as follows: 850 DEG C of solution temperature, use He protection and aerosolization, air pressure 2.67MPa, nozzle diameter
2.16mm.28 μm of obtained powder average diameter, spherical rate > 90%, recovery rate >=55%, TiB2Granule content 5wt.%,
1.4 μm of composite powder average grain size, laser absorption rate 48%.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (9)
1. a kind of preparation method of in-situ Al-base composition, which comprises the steps of:
High temperature covering agent is added in fine aluminium, carries out melting, obtains melt;
KBF is added into the melt4And KTiF6, mix and reacted;
After removing bath surface slag, sequentially add aluminum bronze intermediate alloy, aluminium zirconium hardener, scandium bearing master alloy, in aluminium manganese
Between alloy, aluminium titanium intermediate alloy and pure magnesium, and harmless aluminum refining agent is added, degasification essence is successively carried out at 700~850 DEG C
Refining and aerosolization, obtain in-situ self-generated TiB2The Al-Cu-Mg composite material of particle enhancing.
2. the preparation method of in-situ Al-base composition as described in claim 1, which is characterized in that the aluminum bronze intermediate alloy
For Al-50wt%Cu, aluminium zirconium hardener Al-12wt%Zr, scandium bearing master alloy Al-2wt%Sc, aluminium manganese intermediate alloy
For Al-10wt%Mn, aluminium titanium intermediate alloy is Al-10wt%Ti.
3. the preparation method of in-situ Al-base composition as described in claim 1, which is characterized in that the temperature of the melt is
650~950 DEG C.
4. the preparation method of in-situ Al-base composition as described in claim 1, which is characterized in that the KBF4、K2TiF6's
Mass ratio is 1:(0.5~1:2).
5. the preparation method of in-situ Al-base composition as described in claim 1, which is characterized in that the high temperature covering agent is
JZF-03 type high temperature covering agent.
6. the preparation method of in-situ Al-base composition as described in claim 1, which is characterized in that closed among the aluminum bronze
Gold, aluminium zirconium hardener, scandium bearing master alloy, aluminium manganese intermediate alloy, aluminium titanium intermediate alloy and pure Mg additional amount with aluminium in situ
The metering of element is compared for Al-Cu (0.1%~10%)-Mg (1%~8%)-Zr (0.05%~3%)-Sc in based composites
(0.05%~3%)-Mn (0.05%~2%)-Ti (0.01%~1%) is calculated.
7. the preparation method of in-situ Al-base composition as described in claim 1, which is characterized in that the harmless aluminium alloy essence
Refining agent is JZJ type refining agent.
8. the preparation method of in-situ Al-base composition as described in claim 1, which is characterized in that the condition of the aerosolization
Are as follows: 800~1200 DEG C of melt temperature, aerosolization temperature is 700~850 DEG C, and protection gas is Ar and/or He, air pressure for 1.5~
9.5MPa, nozzle diameter are 0.5~3mm.
9. a kind of preparation method of the in-situ Al-base composition as described in any one of claim 1~8 is in laser gain material
Manufacture the purposes in 2XXX system in-situ Al-base composition.
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