CN115074572A - Preparation method of high-toughness in-situ particle reinforced aluminum alloy matrix composite material - Google Patents

Preparation method of high-toughness in-situ particle reinforced aluminum alloy matrix composite material Download PDF

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CN115074572A
CN115074572A CN202210740180.1A CN202210740180A CN115074572A CN 115074572 A CN115074572 A CN 115074572A CN 202210740180 A CN202210740180 A CN 202210740180A CN 115074572 A CN115074572 A CN 115074572A
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aluminum
powder
melt
aluminum alloy
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陈刚
郑学才
赵玉涛
张振亚
郭盘盘
郝敬存
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Jiangsu University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/06Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-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
    • C22C32/001Non-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 only oxides
    • C22C32/0015Non-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 only oxides with only single oxides as main non-metallic constituents
    • C22C32/0036Matrix based on Al, Mg, Be or alloys thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Abstract

The invention belongs to the technical field of aluminum-based composite materials, and particularly relates to a preparation method of a high-toughness in-situ particle reinforced aluminum alloy-based composite material. The method mixes the dried calcined kaolin with aluminum powder, and ball-milling the mixed powder under the protection of argon in a ball milling tank. Adding the powder into Al-Mn alloy semisolid melt under the mechanical stirring condition, pausing once during stirring, and pressing part of powder floating on the surface of the melt into the melt. Heating and preserving heat after the addition is finished, cooling to a certain temperature, applying corresponding ultrasonic treatment, adding alloy elements to adjust the aluminum alloy matrix3003 component, standing for removing residue, and casting to obtain in-situ Al 2 O 3 A particulate reinforced aluminum matrix composite. The preparation method disclosed by the invention is simple in preparation process, environment-friendly, good in controllability, uniform in distribution of the prepared aluminum matrix composite reinforced particles, clean in interface between the reinforced particles and the matrix, excellent in performance and suitable for large-scale production.

Description

Preparation method of high-toughness in-situ particle reinforced aluminum alloy matrix composite material
Technical Field
The invention belongs to the technical field of aluminum-based composite materials, and particularly relates to a preparation method of a high-toughness in-situ particle reinforced aluminum alloy-based composite material.
Background
3003 aluminum alloy has good corrosion resistance, excellent weldability and excellent press workability due to the addition of Mn, Fe, Si and other elements. It is often used in air conditioners, refrigerators, radiators, etc. However, the 3003 aluminum alloy has lower strength, so that the possibility of thinning the aluminum alloy as a radiating fin is limited, and the subsequent research and improvement are not facilitated. We have investigated the preparation of in situ Al 2 O 3 Particle reinforced 3003 aluminum alloy based composites improve this situation.
The particle reinforced aluminum matrix composite material prepared by the in-situ method has excellent mechanical property, good oxidation resistance and corrosion resistance due to small size of reinforced particles and clean bonding interface with a matrix. Compared with an external method, the bonding strength of the composite material and a matrix interface is higher, and the wettability is better. Therefore, the method has great development prospect in important fields of aerospace, national defense and the like.
The most common reinforcing particles currently used in-situ aluminum-based composite materials are Al 2 O 3 TiC and TiB 2 Etc. of Al 2 O 3 The grain hardness is higher, so that the composite material taking the grain hardness as the reinforcing phase has high specific strength and specific modulus and good wear resistance, and the in-situ Al is used 2 O 3 The particle reinforced aluminum matrix composite material has higher application value.
In recent years, Al has been produced 2 O 3 The particle system is mainly concentrated on Al-ZrO 2 、Al-TiO 2 Al-CuO and Al-SiO 2 Several systems for preparing submicron or nanometer particle reinforced aluminum baseThe price of the raw materials used in the composite material is high, and the cost for preparing the composite material is high. China ranks kaolin mineral resources in the top of the world, has already ascertained 267 mineral production areas and ascertains the reserve volume of 29.10 hundred million tons. The theoretical chemical composition of kaolin is 46.54% SiO 2 39.5% of Al 2 O 3 13.96% of H 2 O, kaolin minerals belong to the 1:1 type phyllosilicates. The kaolin is calcined in a calcining furnace to a certain temperature and time, and the structural water is removed, so that the physical and chemical properties of the kaolin are changed to meet certain use requirements.
The existing in-situ system reaction has some problems, such as particle agglomeration, difficult control of the generated particle size and the like. The mechanical stirring process drives the melt to flow ceaselessly through a stirring device, so that the distribution of internal particles is changed. However, it is difficult to disperse the reactants uniformly in the melt by ordinary mechanical stirring.
Disclosure of Invention
Based on this, the invention aims to provide an in-situ Al 2 O 3 The preparation method of the composite material solves the problems that the strength of the 3003 aluminum alloy is not high and the particles are difficult to disperse.
In order to achieve the purpose, the invention mainly prepares the high-toughness 3003 aluminum alloy-based composite material by a melt reaction method and combining a semi-solid stirring and pressing technology and a high-energy ultrasonic dispersion technology. The method is realized by the following technical scheme: mixing the dried calcined kaolin with aluminum powder, and carrying out ball milling on the mixed powder under the protection of argon in a ball milling tank. Adding the powder into the Al-Mn alloy semi-solid melt under the mechanical stirring condition, pausing once during stirring, and pressing part of the powder floating on the surface of the melt into the Al-Mn alloy semi-solid melt. Heating and preserving heat after adding, cooling to a certain temperature, applying corresponding ultrasonic treatment, adding alloy elements to adjust the aluminum alloy matrix into 3003 components, standing for deslagging, and casting to obtain in-situ Al 2 O 3 A particulate reinforced aluminum matrix composite.
The preparation method comprises the following concrete implementation steps:
(1) mixing the dried calcined kaolin with aluminum powder, placing the mixture into a ball milling tank, and carrying out ball milling under the protection of argon to obtain mixed powder of the aluminum powder and the calcined kaolin, wherein the mass ratio of the aluminum powder to the calcined kaolin is (3-5): 1, ball milling at the rotating speed of 250-350 rpm for 5-10 h;
(2) pure aluminum and Al-20Mn were mixed in a ratio of 30: 2, placing the mixture in a crucible, heating the mixture to 720-730 ℃, keeping the temperature for 10-15 min, degassing the mixed melt of pure aluminum and the Al-Mn intermediate alloy by using a refining agent, and removing redundant slag from the mixed melt;
(3) when the temperature of the mixed melt is reduced to 650-660 ℃, mechanically stirring, adding the mixed powder of the ball-milled aluminum powder and the calcined kaolin into the mixed melt in the stirring process, and continuing to mechanically stir for 2-3 min after the addition is finished;
(4) after stirring, stretching the powder into the aluminum melt from the crucible opening by using a pressing device, pressing the powder with the surface not rolled into the melt, and mechanically stirring for 3-4 min again, wherein the pressing device is a cylindrical graphite disk, and the cylindrical graphite disk is matched with the crucible opening in size, so that the cylindrical graphite disk can be just stretched into the mixed melt;
(5) and heating the mixed melt after adding the mixed powder of the aluminum and the calcined kaolin to 850-900 ℃, and preserving the heat for 30-60 min.
(6) And cooling the mixed melt to 730-750 ℃, and performing dispersion treatment on the mixed melt by using high-energy ultrasonic with the frequency of 15-20 kHz and the power of 500-5000W for 10-15 min.
(7) When the temperature of the mixed melt is reduced to 720-730 ℃, the alloy elements are supplemented to adjust the aluminum alloy matrix component to 3003 aluminum alloy component.
(8) Standing the mixed melt, removing slag, and casting into an iron mold preheated at 250 ℃ to obtain in-situ Al 2 O 3 A particulate reinforced aluminum matrix composite.
For using Al-3Al 2 O 3 ·2SiO 2 Systematic preparation of Al 2 O 3 The aluminum/3003-based composite material is not reported, the invention adds the prefabricated mixed powder into the aluminum melt, the utilization rate of reactant powder is higher, the interface wettability is increased, the reaction is easier, the preparation process is simple, and the green aluminum-based composite material is greenThe color environment-friendly controllability is good, the prepared aluminum matrix composite reinforced particles are uniformly distributed, the interface between the reinforced particles and the matrix is clean, the performance is excellent, and the aluminum matrix composite reinforced particles are suitable for large-scale production.
Drawings
FIG. 1 shows in-situ Al prepared in example 3 2 O 3 The microstructure photograph of the particle reinforced 3003 aluminum alloy based composite material shows that the generated Al 2 O 3 The particles were finer and more uniformly dispersed without significant agglomeration, and both examples 1 and 2 had similar microstructure photographs as example 3.
Table 1 shows the mechanical properties of the 3003 matrix and the composites prepared in the examples.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
Example 1
Finally, 0.5 vol% Al is obtained 2 O 3 /3003 aluminium matrix composite (Al) 2 O 3 The reinforcing particles account for 0.5 vol% of the volume of the finally obtained aluminum matrix composite material) and the preparation process is as follows:
and (2) mixing the dried aluminum powder and calcined kaolin powder according to the mass ratio of 5:1, adding the mixture into a ball mill for ball milling under the protection of argon, wherein the rotating speed is 250r/min, and the ball-material ratio is 10: 1. the ball milling time is 6 h. Drying and preheating the mixed powder after ball milling at 150 ℃ for 2h, melting pure aluminum and Al-Mn intermediate alloy according to the mass ratio of 15:1 at 730 ℃, preserving heat for 15min, and then using a refining agent (C) accounting for 0.3 wt% of the aluminum melt 2 Cl 6 ) Refining and degassing are carried out, and redundant slag is scraped out of the mixed melt. And (3) cooling to 655 ℃ and semi-solid state, adding the mixed powder after ball milling while carrying out mechanical stirring, wherein the rotating speed of a stirring paddle is 800rpm, continuing mechanical stirring for 2min after adding, pressing the powder with the surface not rolled into the melt by using a pressing device, and then carrying out mechanical stirring for 3 min. After the mechanical stirring is finished, heating the melt to 870 ℃, preserving heat for 30min, cooling to 730 ℃, and applying ultrasonic treatment, wherein the ultrasonic frequency is 20kHz, the power is 1kW, and the time isAnd (5) dispersing for 15 min. Supplementing alloy elements after ultrasonic treatment to adjust the components of the aluminum alloy matrix to 3003 aluminum alloy components. Standing the melt for 5min, removing slag, casting the melt into an iron mold preheated to 250 ℃, and cooling to obtain 0.5 vol% Al 2 O 3 A/3003 aluminum matrix composite.
Example 2
Finally obtaining 1 vol% Al 2 O 3 The preparation process of the/3003 aluminum matrix composite material is as follows:
and (2) mixing the dried aluminum powder and calcined kaolin powder according to a mass ratio of 4: 1, adding the mixture into a ball mill for ball milling under the protection of argon, wherein the rotating speed is 250r/min, and the ball-material ratio is 10: 1. the ball milling time is 8 h. Drying and preheating the mixed powder after ball milling at 150 ℃ for 2h, melting pure aluminum and Al-Mn intermediate alloy according to the mass ratio of 15:1 at 730 ℃, preserving heat for 15min, and then using a refining agent (C) accounting for 0.3 wt% of the aluminum melt 2 Cl 6 ) Refining and degassing are carried out, and redundant slag is scraped out from the mixed melt. And (3) cooling to 655 ℃ and semi-solid state, adding the mixed powder after ball milling while carrying out mechanical stirring, wherein the rotating speed of a stirring paddle is 1000rpm, continuing mechanical stirring for 2min after adding, pressing the powder with the surface not rolled into the melt by using a pressing device, and then carrying out mechanical stirring for 4 min. After the mechanical stirring is finished, heating the melt to 870 ℃, preserving heat for 40min, cooling to 730 ℃, applying ultrasonic treatment, wherein the ultrasonic frequency is 20kHz, the power is 1kW, and the time is 15min, and performing dispersion treatment on the melt. Supplementing alloy elements after ultrasonic treatment to adjust the components of the aluminum alloy matrix to 3003 aluminum alloy components. Standing the melt for 5min, removing slag, casting into an iron mold preheated to 250 ℃, and cooling to obtain 1 vol% Al 2 O 3 A/3003 aluminum matrix composite.
Example 3
Finally obtaining 1.5 vol% Al 2 O 3 The preparation process of the/3003 aluminum matrix composite material is as follows:
and (2) mixing the dried aluminum powder and calcined kaolin powder according to the mass ratio of 3: 1, adding the mixture into a ball mill for ball milling under the protection of argon, wherein the rotating speed is 250r/min, and the ball-material ratio is 10: 1. the ball milling time is 10 h. To the mixed powder after ball millingDrying and preheating at 150 ℃ for 2h, melting pure aluminum and Al-Mn intermediate alloy according to the mass ratio of 15:1 at 730 ℃, preserving heat for 15min, and then using a refining agent (C) accounting for 0.3 wt% of the aluminum melt 2 Cl 6 ) Refining and degassing are carried out, and redundant slag is scraped out from the mixed melt. And (3) cooling to 655 ℃ and semi-solid state, adding the mixed powder after ball milling while carrying out mechanical stirring, wherein the rotating speed of a stirring paddle is 1200rpm, continuing mechanical stirring for 3min after adding, pressing the powder with the surface not rolled into the melt by using a pressing device, and then carrying out mechanical stirring for 4 min. After the mechanical stirring is finished, heating the melt to 870 ℃, preserving heat for 50min, cooling to 730 ℃, applying ultrasonic treatment, wherein the ultrasonic frequency is 20kHz, the power is 1kW, and the time is 15min, and performing dispersion treatment on the melt. Supplementing alloy elements after ultrasonic treatment to adjust the components of the aluminum alloy matrix to 3003 aluminum alloy components. Standing the melt for 5min, removing slag, casting into an iron mold preheated to 250 ℃, and cooling to obtain 1.5 vol% Al 2 O 3 A/3003 aluminum matrix composite.
TABLE 1
Figure BDA0003717586420000041
Figure BDA0003717586420000051

Claims (8)

1. A preparation method of a high-toughness in-situ particle reinforced aluminum alloy matrix composite material is characterized by comprising the following specific steps:
(1) mixing the dried calcined kaolin with aluminum powder, placing the mixture into a ball milling tank, and carrying out ball milling under the protection of argon to obtain mixed powder of the aluminum powder and the calcined kaolin, wherein the mass ratio of the aluminum powder to the calcined kaolin is 3-5: 1;
(2) pure aluminum and Al-20Mn are mixed according to the ratio of 30: 2, placing the mixture in a crucible, heating the mixture to 720-730 ℃, keeping the temperature, degassing the mixed melt of the pure aluminum and the Al-Mn intermediate alloy by using a refining agent, and removing redundant slag from the mixed melt;
(3) when the temperature of the mixed melt is reduced to 650-660 ℃, mechanically stirring, adding the mixed powder of the ball-milled aluminum powder and the calcined kaolin into the mixed melt in the stirring process, and continuing to mechanically stir after the addition is finished;
(4) after stirring, extending the powder into the aluminum melt from the crucible opening by using a pressing device, pressing the powder which is not rolled into the surface into the melt, and mechanically stirring again;
(5) heating the mixed melt after adding the mixed powder of aluminum and calcined kaolin to 850-900 ℃ and preserving heat;
(6) cooling the mixed melt to 730-750 ℃, and dispersing the mixed melt by using high-energy ultrasound;
(7) when the temperature of the mixed melt is reduced to 720-730 ℃, supplementing alloy elements to adjust the aluminum alloy matrix component to a 3003 aluminum alloy component;
(8) standing the mixed melt, removing slag, and casting into a preheated iron mold to obtain in-situ Al 2 O 3 A particulate reinforced aluminum matrix composite.
2. The preparation method of the high-toughness in-situ particle reinforced aluminum alloy-based composite material as claimed in claim 1, wherein in the step (1), the ball milling rotation speed is 250-350 rpm, and the ball milling time is 5-10 h.
3. The preparation method of the high-toughness in-situ particle reinforced aluminum alloy matrix composite material as claimed in claim 1, wherein in the step (2), the heat preservation time is 10-15 min.
4. The preparation method of the high-toughness in-situ particle reinforced aluminum alloy-based composite material as claimed in claim 1, wherein in the step (3), the time for continuing mechanical stirring is 2-3 min.
5. The preparation method of the high-toughness in-situ particle reinforced aluminum alloy matrix composite material as claimed in claim 1, wherein in the step (4), the time for mechanical stirring again is 3-4 min; the pressing equipment is a cylindrical graphite plate, and the cylindrical graphite plate is matched with the size of the crucible opening, so that the cylindrical graphite plate can just stretch into the mixed melt.
6. The preparation method of the high-toughness in-situ particle reinforced aluminum alloy-based composite material as claimed in claim 1, wherein in the step (5), the heat preservation time is 30-60 min.
7. The preparation method of the high-toughness in-situ particle reinforced aluminum alloy matrix composite material as claimed in claim 1, wherein in the step (6), the high-energy ultrasonic frequency is 15-20 kHz, the power is 500-5000W, and the dispersion treatment time is 10-15 min.
8. The method for preparing the high-toughness in-situ particle reinforced aluminum alloy matrix composite material as claimed in claim 1, wherein in the step (8), the preheating temperature of the iron mold is 250 ℃.
CN202210740180.1A 2022-06-28 2022-06-28 Preparation method of high-toughness in-situ particle reinforced aluminum alloy matrix composite material Pending CN115074572A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116043059A (en) * 2023-01-18 2023-05-02 江苏大学 Method for preparing micro-nano particle hybrid reinforced aluminum matrix composite
CN117418132A (en) * 2023-12-18 2024-01-19 阜新中孚轻金属科技有限公司 Al (aluminum) alloy 2 O 3 Preparation method of/A356 composite material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3860416A (en) * 1972-08-02 1975-01-14 Ethyl Corp Modified aluminum process
CN111663061A (en) * 2020-06-23 2020-09-15 江苏大学 Method for preparing Al-Si alloy grain refiner

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3860416A (en) * 1972-08-02 1975-01-14 Ethyl Corp Modified aluminum process
CN111663061A (en) * 2020-06-23 2020-09-15 江苏大学 Method for preparing Al-Si alloy grain refiner

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116043059A (en) * 2023-01-18 2023-05-02 江苏大学 Method for preparing micro-nano particle hybrid reinforced aluminum matrix composite
CN117418132A (en) * 2023-12-18 2024-01-19 阜新中孚轻金属科技有限公司 Al (aluminum) alloy 2 O 3 Preparation method of/A356 composite material

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Application publication date: 20220920