CN107794395B - Melt controls the preparation method of spontaneous aluminum matrix composite - Google Patents
Melt controls the preparation method of spontaneous aluminum matrix composite Download PDFInfo
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- CN107794395B CN107794395B CN201610757301.8A CN201610757301A CN107794395B CN 107794395 B CN107794395 B CN 107794395B CN 201610757301 A CN201610757301 A CN 201610757301A CN 107794395 B CN107794395 B CN 107794395B
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 42
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000011159 matrix material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 230000002269 spontaneous effect Effects 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 150000003839 salts Chemical class 0.000 claims abstract description 20
- 229910052786 argon Inorganic materials 0.000 claims abstract description 13
- 239000004411 aluminium Substances 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005266 casting Methods 0.000 claims abstract description 5
- 239000000956 alloy Substances 0.000 claims abstract description 4
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 4
- 238000007670 refining Methods 0.000 claims abstract description 4
- 239000002893 slag Substances 0.000 claims abstract description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 10
- 239000000155 melt Substances 0.000 claims description 10
- 229910052749 magnesium Inorganic materials 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- 229910020808 NaBF Inorganic materials 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 229910033181 TiB2 Inorganic materials 0.000 abstract description 14
- 238000009826 distribution Methods 0.000 abstract description 8
- 238000005204 segregation Methods 0.000 abstract description 8
- 239000008187 granular material Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 19
- 239000002245 particle Substances 0.000 description 19
- 238000000034 method Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 238000004062 sedimentation Methods 0.000 description 9
- 230000002787 reinforcement Effects 0.000 description 7
- 230000035484 reaction time Effects 0.000 description 6
- 239000011833 salt mixture Substances 0.000 description 6
- 229910001610 cryolite Inorganic materials 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- 238000007664 blowing Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 229910001495 sodium tetrafluoroborate Inorganic materials 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The present invention provides the preparation method that a kind of melt controls spontaneous aluminum matrix composite, include the following steps: that reacting salt and reaction promoter is added, is blown into argon gas and stirs, reacts by after fine aluminium or alloy matrix aluminum fusing；After the reaction was completed remove salt slag, carry out refining treatment after casting to get.The preparation method solves aluminum matrix composite TiB2The problems such as size of reinforced phase and distribution are controllable and settle segregation.It is prepared for TiB2Granule content is up to 15%wt and the aluminum matrix composite of even tissue and function admirable, while the further expansion application for also preparing particulate reinforced composite for mixing salts reaction provides foundation.
Description
Technical field
The invention belongs to field of compound material, are related to a kind of method for preparing aluminum matrix composite, and in particular, to a kind of
Melt controls the preparation method of spontaneous aluminum matrix composite.
Background technique
In recent years, many articles have reported the research about in-situ authigenic reaction particles reinforced aluminum matrix composites.It is special
Point is: enhancing particle combines preferable and clean interfaces in intrinsic silicon fabricated in situ, basal body interface；In-sltu reinforcement finer grain size
Small (generally < 3.0 μm) and be evenly distributed in the base；By selection reaction type and control response parameter, can get not of the same race
The In-sltu reinforcement particle of class, different number；The fabricated in situ of enhancing particle combines with foundry engieering；Simple process, cost
It is low；It can be used to prepare the composite material of certain shapes and size.It finds by literature search, Dacies P.Development of
Cast Aluminium MMCs (development of aluminum matrix composite), Key Engineering Materials (important engineering material
Material), 1993,77:357-362, but this method there is reinforced phase particle size in prepared composite material and is unevenly distributed
It is even；And mass fraction is not high, or works as TiB2When mass fraction is greater than 8wt%, institutional framework deteriorates, and casting character is deteriorated, material
The mechanical property of material substantially reduces.How size, distribution and the sedimentation segregation of reinforced phase are effectively controlled using reasonable technique
It there are no report always.
Summary of the invention
For the defects in the prior art, the object of the present invention is to provide a kind of melts to control spontaneous aluminum matrix composite
Preparation method solves aluminum matrix composite TiB2The problems such as size of reinforced phase and distribution are controllable and settle segregation.
The purpose of the present invention is what is be achieved through the following technical solutions:
For the present invention by the way that reaction adjuvant and multi- scenarios method technique containing melt alloying element is added, control reaction is auxiliary
Type, additional amount, proportion, mixing speed, the reaction temperature of addition and the reaction time of auxiliary agent and pulsed magnetic field and high energy are super
The intensity collective effect of sound field, to realize reinforced phase TiB2The size of particle and distribution are controllable, and solve aluminum matrix composite
The sedimentation segregation problem of melt, and then prepare the aluminum matrix composite of even tissue and function admirable.
The present invention provides the preparation methods that a kind of melt controls spontaneous aluminum matrix composite, include the following steps:
After fine aluminium or alloy matrix aluminum fusing, reacting salt and reaction promoter is added, is blown into argon gas and stirs, reacts；
After the reaction was completed remove salt slag, carry out refining treatment after casting to get.
Preferably, the preparation method further includes that the magnesium of 1-2wt% is added in the melt by after matrix melts.
Preferably, the reaction promoter includes the Na that mass ratio is 2:1:1~4:1:13AlF6、LiF3、LiCl3。
Preferably, the reacting salt includes the NaBF that mass ratio is 1:1~2:14And Na2TiF6。
Preferably, the additional amount of the reaction promoter is the 5-15wt% of reacting salt l.The additional amount of reaction promoter is excessively high,
It will lead to also uneconomical in the combined coefficient reduction and cost control of reaction；Additional amount is too low, will lead to the TiB of generation2Particle
Size distribution is discrete, and uniformity is poor.
Preferably, the argon flow is 5~15L/min, and speed of agitator is 250~350r/min.
Preferably, in the reaction process, apply the pulsed magnetic field intensity of 1-5T.
Preferably, in the reaction process, apply 50-2000W/m2High-energy ultrasonic field intensity.
Preferably, the reaction time is 10min~30min.
Preferably, the addition temperature of the reaction promoter is 720~760 DEG C.
Preferably, the reaction promoter is sufficiently mixed uniformly before addition and dries.
The present invention controls reinforced phase TiB2Size and distribution, it is important to solve dynamics process in reaction process.Anti-
During answering, melt temperature is controlled in relatively narrow temperature range, and apply pulsed magnetic field and high-energy ultrasonic field simultaneously.
Solve TiB2The sedimentation segregation problem of reinforced aluminum matrix composites, key point are how to prevent TiB2Particle is logical
Itself is crossed to reunite to drop low-surface-energy.Suitable magnesium metal (content is about 1-2%) is added in the composite, makes particles generation
Low-surface-energy is dropped by the magnesium in absorption molten aluminum first afterwards, then forms preferable combination with aluminium again, in this way using magnesium as
The phenomenon that reducing particle surface energy, prevent the means reunited, effectively slowing down particle sedimentation.Simultaneously because the addition of magnesium, makes
The viscosity of molten aluminum increases, and according to Stocks formula, composite emulsion viscosities increase, and the movement speed of particle reduces, when longer
It is interior to reunite because contacting with each other, it is also easy to be captured by the crystal grain of α-Al in process of setting, forms stable homogeneous
Reinforcement.
Usual generated in-situ TiB2Particle is the particle that diameter is 1 microns, and the particle of this size is in molten aluminum
The appearance of sedimentation is not had.But since particle is often generated at a certain regional area (on fused salt and the interface of molten aluminum), very
It is easy to reunite because local concentration is higher.And once reunite and generate, then it is made separately to refine just very difficulty, in
It is the segregation just having in sedimentation and process of setting.Using pulsed magnetic field and high-energy ultrasonic field is applied, melted using reaction
The protective effect of salt itself, by pulsed magnetic field intensity control in 1-5T, high-energy ultrasonic field intensity is controlled in 50-2000W/m2.One
Aspect can increase the touch opportunity of fused salt and molten aluminum, accelerate reaction, make generated in-situ TiB2Particle is uniformly tiny；Another party
Face promotes diffusion of the particle from the high concentration region of reaction to low concentration region, makes TiB2Particle is uniformly and disperse, and then but also multiple
The sedimentation phenomenon of condensation material has obtained certain alleviation.
The prior art is compared, and the present invention has following the utility model has the advantages that the present invention is by melt alloying element and more
Coupling technique solves TiB2Size, distribution and the sedimentation segregation problem of reinforced phase, are prepared for TiB2Granule content is up to 15%
Wt and the excellent aluminum matrix composite of structure property, while also further opening up for particulate reinforced composite is prepared for salts reaction
Exhibition application provides foundation.
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.
The preparation method that a kind of melt controls spontaneous aluminum matrix composite is provided in the embodiment of the present invention, including as follows
Step:
Fine aluminium or alloy matrix aluminum are melted in 700~760 DEG C of temperature ranges, while keeping the temperature homogenization 20min, is added anti-
Salt and reaction promoter are answered, using rotary blowing argon gas and is stirred, is reacted；
After the reaction was completed remove salt slag, carry out refining treatment after casting to get.
The preparation method further includes that the magnesium of 1-2wt% is added in the melt by after matrix melts.
The reaction promoter includes the Na that mass ratio is 2:1:1~4:1:13AlF6、LiF3、LiCl3。
The reacting salt includes the NaBF that mass ratio is 1:1~2:14And Na2TiF6。
The additional amount of the reaction promoter is the 5-15wt% of reacting salt.
The argon flow is 5~15L/min, and speed of agitator is 250~350r/min.
In the reaction process, apply the pulsed magnetic field intensity of 1-5T.
In the reaction process, apply 50-2000W/m2High-energy ultrasonic field intensity.
The reaction time is 10min~30min.
The addition temperature of the reaction promoter is 720~760 DEG C.
The reaction promoter is sufficiently mixed uniformly before addition and dries.
Embodiment 1
The magnesium of 1wt% is added using fine aluminium as basis material in the present embodiment in the melt, and mass ratio is the NaBF of 1:14With
Na2TiF6As reaction salt-mixture, and it is aided with Na3AlF6、LiF3、LiCl3Make reaction promoter, proportion is 2:1:1, reaction promoter
Gross mass is react salt-mixture 10%, and reaction promoter is added 760 DEG C of temperature, and the reaction time is 30min；Rotary blowing argon gas is applied
With stirring, rotor speed 300r/min, argon flow 10L/min；Pulsed magnetic field intensity is controlled in 1.5T, high-energy ultrasonic field intensity
Control is in 200W/m2, prepare the TiB that mass percent is 14wt%2In-sltu reinforcement fine aluminium composite material.The as cast condition as cast condition of material
Mechanical property: σb=180Mpa；σ0.2=112Mpa；δ=7.8%；E=88.7Gpa.
Embodiment 2
The magnesium of 2wt% is added using ZL101 as basis material in the present embodiment in the melt, and mass ratio is 1.5:1's
NaBF4And Na2TiF6As reaction salt-mixture, and it is aided with Na3AlF6、LiF3、LiCl3Make reaction promoter, proportion is 3:1:1,
Reaction promoter gross mass is react salt-mixture 15%；Reaction promoter is added 720 DEG C of temperature, and the reaction time is 20min；Rotation spray
Blowing argon gas imposes stirring, rotor speed 250r/min, argon flow 5L/min；In 2.5T, high energy is super for pulsed magnetic field intensity control
Sound field intensity is controlled in 500W/m2, prepare the TiB that mass percent is 10wt%2/ ZL101 composite material.The as cast condition of material is cast
State mechanical property: σb=265Mpa；σ0.2=213Mpa；δ=2.8%；E=83.2Gpa.
Embodiment 3
The magnesium of 1.5wt% is added using ZL109 as basis material in the present embodiment in the melt, and mass ratio is 2:1's
NaBF4And Na2TiF6As reaction salt-mixture, and it is aided with Na3AlF6、LiF3、LiCl3Make reaction promoter, proportion is 4:1:1,
Reaction promoter gross mass is react salt-mixture 5%；Reaction promoter is added 740 DEG C of temperature, and the reaction time is 30min；Rotation spray
Blowing argon gas imposes stirring, rotor speed 350r/min, argon flow 15L/min；Pulsed magnetic field intensity is controlled in 2T, high-energy ultrasonic
Field intensity is controlled in 800W/m2, prepare the TiB that mass percent is 15wt%2/ ZL109 composite material.The as cast condition as cast condition of material
Mechanical property: σb=268Mpa；σ0.2=206Mpa；δ=1.7%；E=91.8Gpa.
Comparative example 1
The preparation method of this comparative example is same as Example 1, the difference is that only: Na3AlF6、LiF3、LiCl3Match
Than for 1:2:1.Prepare the TiB that mass percent is 14wt%2In-sltu reinforcement fine aluminium composite material.The as cast condition as cast condition power of material
Learn performance: σb=152Mpa；σ0.2=100Mpa；δ=6.5%；E=86.5Gpa.
Comparative example 2
The preparation method of this comparative example is same as Example 1, the difference is that only: Na3AlF6、LiF3、LiCl3Match
Than for 5:1:2.Prepare the TiB that mass percent is 14wt%2In-sltu reinforcement fine aluminium composite material.The as cast condition as cast condition power of material
Learn performance: σb=157Mpa；σ0.2=105Mpa；δ=6.8%；E=86.1Gpa.
Comparative example 3
The preparation method of this comparative example is same as Example 1, the difference is that only: reaction promoter gross mass is that reaction is mixed
Close the 20% of salt.Prepare the TiB that mass percent is 14wt%2In-sltu reinforcement fine aluminium composite material.The as cast condition as cast condition of material
Mechanical property: σb=142Mpa；σ0.2=101Mpa；δ=6.0%；E=85.7Gpa.
Comparative example 4
The preparation method of this comparative example is same as Example 2, the difference is that only: not applying pulsed magnetic field.It prepares
Mass percent is the TiB of 10wt%2/ ZL101 composite material.The as cast condition as cast condition mechanical property of material: σb=235Mpa；σ0.2=
183Mpa；δ=2.2%；E=81.7Gpa.
Comparative example 5
The preparation method of this comparative example is same as Example 2, the difference is that only: not applying high-energy ultrasonic field.Preparation
Mass percentage is the TiB of 10wt%2/ ZL101 composite material.The as cast condition as cast condition mechanical property of material: σb=220Mpa；σ0.2
=175Mpa；δ=1.8%；E=82.0Gpa.
In conclusion the present invention solves TiB by melt alloying element and multi- scenarios method technique2The size of reinforced phase,
Distribution and sedimentation segregation problem, are prepared for TiB2Granule content is up to 15%wt and the excellent aluminum-base composite material of structure property
Material, while the further expansion application for also preparing particulate reinforced composite for salts reaction provides foundation.
There are many concrete application approach of the present invention, the above is only a preferred embodiment of the present invention.More than it should be pointed out that
Embodiment is merely to illustrate the present invention, and the protection scope being not intended to restrict the invention.For the common skill of the art
For art personnel, without departing from the principle of the present invention, several improvement can also be made, these improvement also should be regarded as this hair
Bright protection scope.
Claims (5)
1. the preparation method that a kind of melt controls spontaneous aluminum matrix composite, which comprises the steps of:
After fine aluminium or alloy matrix aluminum fusing, reacting salt and reaction promoter is added, is blown into argon gas and stirs, reacts；
After the reaction was completed remove salt slag, carry out refining treatment after casting to get；
The reaction promoter includes the Na that mass ratio is 2:1:1~4:1:13AlF6、LiF3、LiCl3；
The reacting salt includes the NaBF that mass ratio is 1:1~2:14And Na2TiF6；
The additional amount of the reaction promoter is the 5-15wt% of reacting salt；
The preparation method further includes that the magnesium of 1-2wt% is added in the melt by after matrix melts；
In the reaction process, apply the pulsed magnetic field intensity of 1-5T；
In the reaction process, apply 50-2000W/m2High-energy ultrasonic field intensity.
2. the preparation method that melt according to claim 1 controls spontaneous aluminum matrix composite, which is characterized in that the argon
Throughput is 5~15L/min, and speed of agitator is 250~350r/min.
3. the preparation method that melt according to claim 1 controls spontaneous aluminum matrix composite, which is characterized in that described anti-
It is 10min~30min between seasonable.
4. the preparation method that melt according to claim 1 controls spontaneous aluminum matrix composite, which is characterized in that described anti-
The addition temperature for answering auxiliary agent is 720~760 DEG C.
5. the preparation method that melt according to claim 1 controls spontaneous aluminum matrix composite, which is characterized in that described anti-
It answers auxiliary agent to be sufficiently mixed before addition uniformly and dries.
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| CN112795804B (en) * | 2020-12-27 | 2021-11-09 | 上海交通大学安徽(淮北)陶铝新材料研究院 | Method for controlling in-situ authigenic aluminum-based composite material by melt with continuous treatment |
| CN112779435B (en) * | 2020-12-27 | 2021-12-14 | 上海交通大学安徽(淮北)陶铝新材料研究院 | Method for controlling in-situ authigenic aluminum-based composite material through melt with electromagnetic stirring |
| CN112795805B (en) * | 2020-12-27 | 2021-11-19 | 上海交通大学安徽(淮北)陶铝新材料研究院 | Preparation method of in-situ autogenous aluminum-based composite material with powder injection |
| CN112779433B (en) * | 2020-12-27 | 2021-12-21 | 上海交通大学安徽(淮北)陶铝新材料研究院 | Argon gas rotary blowing and raw material synchronous conveying method for in-situ autogenous aluminum-based composite material preparation |
| CN112760505B (en) * | 2020-12-27 | 2022-04-29 | 上海交通大学安徽(淮北)陶铝新材料研究院 | In-situ autogenous aluminum matrix composite material system with vacuum degassing |
| CN112760518B (en) * | 2020-12-27 | 2021-11-30 | 上海交通大学安徽(淮北)陶铝新材料研究院 | Method for in-situ self-growing aluminum-based composite material with vacuum degassing |
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| CN102121075A (en) * | 2011-02-15 | 2011-07-13 | 江苏大学 | Method for synthesizing particle reinforced aluminum-based composite under high-intensity ultrasonic field and pulsed electric field |
| CN104264001A (en) * | 2014-09-16 | 2015-01-07 | 广东新劲刚新材料科技股份有限公司 | In-situ synthesized particle reinforced aluminum matrix composite material and preparation method thereof |
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