CN109082568A - A kind of fabricated in situ nanometer CuAl2/Al2O3The preparation method of reinforced aluminum matrix composites - Google Patents

A kind of fabricated in situ nanometer CuAl2/Al2O3The preparation method of reinforced aluminum matrix composites Download PDF

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Publication number
CN109082568A
CN109082568A CN201810997554.1A CN201810997554A CN109082568A CN 109082568 A CN109082568 A CN 109082568A CN 201810997554 A CN201810997554 A CN 201810997554A CN 109082568 A CN109082568 A CN 109082568A
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powder
mixed
ball
milling
aluminum matrix
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CN201810997554.1A
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Inventor
赵乃勤
戎旭东
何春年
师春生
何芳
马丽颖
刘恩佐
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Tianjin University
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Tianjin University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/12Alloys based on aluminium with copper as the next major constituent
    • 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
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/058Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention relates to a kind of fabricated in situ nanometer CuAl2/Al2O3The preparation method of reinforced aluminum matrix composites, including the following steps: (1) prepare mixed-powder, according to cupric oxide powder: aluminium powder or Al alloy powder mass ratio are to weigh mixed-powder less than 10%.(2) ball-milling treatment is carried out to mixed-powder, mixed-powder is fitted into spheroidal graphite tank, ball-milling treatment is carried out to mixed-powder under protection of argon gas, ball milling parameter: ratio of grinding media to material 5:1~15:1, revolving speed 200r/min, Ball-milling Time 1~4 hour.(3) sinter molding.

Description

A kind of fabricated in situ nanometer CuAl2/Al2O3The preparation method of reinforced aluminum matrix composites
Technical field
Powder metallurgical technique fabricated in situ nanometer CuAl is utilized the present invention relates to a kind of2/Al2O3Enhance aluminum-base composite material The method of material belongs to metal-base composites preparation technical field.
Background technique
Aluminum matrix composite due to having many advantages, such as that specific strength is high, electrical and thermal conductivity performance is good, be widely used in aerospace and Civil field.It mostly uses ceramic particle, ceramic whisker, spinel particle etc. as reinforced phase in traditional aluminum matrix composite, draws Enter the method for reinforced phase then mainly using outer addition.However in the design of the above composite system and technology of preparing, there are several The shortcomings that aspect.It introduces reinforced phase by outer addition first to will lead to that reinforced phase is unevenly distributed, reinforced phase introduces opposite and contain It measures lower, poor with matrix associativity.In addition, excessive ceramic phase is introduced into aluminum substrate, due to the thermal expansion of itself and matrix Coefficient mismatches, and is easy to cause composite material to crack during military service.Introducing reinforced phase using in-situ method then can be effective gram Disadvantage mentioned above is taken, the preferable aluminum matrix composite of comprehensive mechanical property is conducive to.
Make reducing agent with aluminium, metal oxide can pass through original position as oxidant, by thermit reaction in aluminum substrate It reacts a step and obtains intermetallic compound and aluminium oxide.Intermetallic compound not only intensity with higher, while and aluminum substrate Interface bond strength is higher, and the aluminium oxide generated can also be used as the reinforcement in aluminum matrix composite.But due to causing aluminium The energy barrier of thermal response is higher, therefore previous researcher realizes thermit reaction through the mode frequently with casting.But it cast Since thermit reaction is more violent thermal explosion can often occur for Cheng Zhong, lead to experimentation danger with higher, need to develop one The new reactive mode of kind.
Summary of the invention
The purpose of the present invention is to provide one kind to prepare CuAl by fabricated in situ mode2/Al2O3Enhance aluminum-base composite material The method of material, this method can reduce risk, and can effectively overcome reinforced phase cyrystal boundary segregation in casting, be unevenly distributed The shortcomings that.To achieve the above object, the present invention is implemented by the following technical programs:
A kind of fabricated in situ nanometer CuAl2/Al2O3The preparation method of reinforced aluminum matrix composites, including the following steps:
(1) mixed-powder is prepared
According to cupric oxide powder: aluminium powder or Al alloy powder mass ratio are to weigh mixed-powder less than 10%.
(2) ball-milling treatment is carried out to mixed-powder
Mixed-powder is fitted into spheroidal graphite tank, ball-milling treatment, ball milling parameter: ball are carried out to mixed-powder under protection of argon gas Material is than 5:1~15:1, revolving speed 200r/min, and Ball-milling Time 1~4 hour.
(3) sinter molding.
Reaction mechanism: although cupric oxide powder itself has very high fusing point, when it forms mixed powder opisthosoma with aluminium powder When being, aluminium powder may act as reducing agent, and cupric oxide powder may act as oxidant.And guaranteeing two kinds of powder by way of ball milling Higher energy is also inputted while uniformly mixed into system, it is thus possible to promote the mixed-powder system can be in aluminium fusing point It is reacted below.Reaction equation: CuO+Al → CuAl2+Al2O3
Detailed description of the invention
Fig. 1 is original aluminium powder pattern
Fig. 2 is native oxide copper powder pattern
Fig. 3 is that ball milling mixes pattern after powder
Fig. 4 is cold pressing block DSC-TG curve
Fig. 5 is tissue topography of the composite material under scanning electron microscope and transmission electron microscope after sintering, a) is aoxidized at granular boundary Aluminium;B) TEM crystal boundary;C) nanometer CuAl under TEM2;D) nanometer Al under TEM2O3Particle
Fig. 6 is engineering stress-strain curve of the fine aluminium of hot pressing state composite material and same process preparation.
Specific embodiment
Technology path of the invention is as follows:
(1) mixed-powder is prepared
According to cupric oxide powder: aluminium powder (or Al alloy powder) mass ratio is to weigh mixed-powder less than 10%.
(2) ball-milling treatment is carried out to mixed-powder
Mixed-powder is fitted into spheroidal graphite tank, ball-milling treatment, ball milling parameter: ball are carried out to mixed-powder under protection of argon gas Material is than 5:1~15:1, revolving speed 200r/min, and Ball-milling Time 1~4 hour.
(3) sinter molding
Powder after ball milling, which is put into the mold of vacuum hotpressing stove, carries out Thermocompressed sintering and forming, sintering pressure 50MPa, burns Junction temperature is 620 DEG C.The pressure sintering process such as HIP sintering, discharge plasma sintering is used equally for powder sintered molding. The composite material of preparation can further increase material property by subsequent heat processing technique.
It further illustrates that the present invention, these examples are served only for illustrating the present invention below with reference to example, is not intended to limit the present invention.
Embodiment 1
It weighs 19.8g aluminium powder (as shown in Figure 1), 0.2g cupric oxide powder (as shown in Figure 2), 0.2g stearic acid (is used as process Controlling agent prevents that cold welding occurs in mechanical milling process), it is placed in 250 milliliters of stainless steel jar mill, and be filled with argon gas.Using row Planetary ball mill was with 200r/min ball milling 2 hours, ratio of grinding media to material 15:1.The mixed-powder after ball milling is taken out in vacuum glove box (as shown in Figure 3).For Wen Di required for precise measurement hot pressed sintering, the powder after ball milling mixing is cold-pressed as block first, DSC-TG test is carried out to the block after cold pressing.Diameter is then used to carry out vacuum heating-press sintering, sintering temperature for the mold of 45mm 620 DEG C of degree, sintering pressure 50MPa.Obtain the nanometer CuAl that diameter is 45mm thickness about 4mm2/Al2O3Enhance aluminum-base composite material Expect sample (as shown in Figure 5).
It by linear cutter is the style that can be used for stretching by aluminum matrix composite, using universal tensile testing machine It is stretched, rate of extension 0.5mm/min, it is as shown in Figure 6 which stretches engineering stress strain curve
Embodiment 2
19.8g aluminium powder, 0.4g cupric oxide powder are weighed, 0.2g stearic acid (is used as process control agent, prevents from sending out in mechanical milling process Raw food weldering), it is placed in 250 milliliters of stainless steel jar mill, and be filled with argon gas.Use planetary ball mill with 200r/min ball Mill 2 hours, ratio of grinding media to material 15:1.In vacuum glove box take out ball milling after mixed-powder, use diameter for the mold of 45mm into Row vacuum heating-press sintering, 620 DEG C of sintering temperature, sintering pressure 50MPa.Obtain the nanometer that diameter is 45mm thickness about 4mm CuAl2/Al2O3Reinforced aluminum matrix composites sample.
It by linear cutter is the style that can be used for stretching by aluminum matrix composite, using universal tensile testing machine It is stretched, rate of extension 0.5mm/min, obtains the composite material and stretch engineering stress strain curve.
Embodiment 3
19.8g aluminium powder, 0.6g cupric oxide powder are weighed, 0.2g stearic acid (is used as process control agent, prevents from sending out in mechanical milling process Raw food weldering), it is placed in 250 milliliters of stainless steel jar mill, and be filled with argon gas.Use planetary ball mill with 200r/min ball Mill 2 hours, ratio of grinding media to material 15:1.In vacuum glove box take out ball milling after mixed-powder, use diameter for the mold of 45mm into Row vacuum heating-press sintering, 620 DEG C of sintering temperature, sintering pressure 50MPa.Obtain the nanometer that diameter is 45mm thickness about 4mm CuAl2/Al2O3Reinforced aluminum matrix composites sample.
It by linear cutter is the style that can be used for stretching by aluminum matrix composite, using universal tensile testing machine It is stretched, rate of extension 0.5mm/min, obtains the composite material and stretch engineering stress strain curve.
Embodiment 4
19.8g aluminium powder, 0.8g cupric oxide powder are weighed, 0.2g stearic acid (is used as process control agent, prevents from sending out in mechanical milling process Raw food weldering), it is placed in 250 milliliters of stainless steel jar mill, and be filled with argon gas.Use planetary ball mill with 200r/min ball Mill 2 hours, ratio of grinding media to material 15:1.In vacuum glove box take out ball milling after mixed-powder, use diameter for the mold of 45mm into Row vacuum heating-press sintering, 620 DEG C of sintering temperature, sintering pressure 50MPa.Obtain the nanometer that diameter is 45mm thickness about 4mm CuAl2/Al2O3Reinforced aluminum matrix composites sample.
It by linear cutter is the style that can be used for stretching by aluminum matrix composite, using universal tensile testing machine It is stretched, rate of extension 0.5mm/min, obtains the composite material and stretch engineering stress strain curve.
Embodiment 5
19.8g aluminium powder, 1g cupric oxide powder are weighed, 0.2g stearic acid (is used as process control agent, prevents from occurring in mechanical milling process Cold welding), it is placed in 250 milliliters of stainless steel jar mill, and be filled with argon gas.Use planetary ball mill with 200r/min ball milling 2 Hour, ratio of grinding media to material 15:1.The mixed-powder after ball milling is taken out in vacuum glove box, uses diameter to carry out for the mold of 45mm true Empty hot pressed sintering, 620 DEG C of sintering temperature, sintering pressure 50MPa.Obtain the nanometer CuAl that diameter is 45mm thickness about 4mm2/ Al2O3Reinforced aluminum matrix composites sample.
It by linear cutter is the style that can be used for stretching by aluminum matrix composite, using universal tensile testing machine It is stretched, rate of extension 0.5mm/min, obtains the composite material and stretch engineering stress strain curve.
Aluminium powder and cupric oxide powder are uniformly mixed in such a way that ball milling mixes powder, pass through the side of powder metallurgy by the present invention Method is in aluminium fusing point following implemented thermit reaction, fabricated in situ nanometer CuAl2/Al2O3Reinforced aluminum matrix composites.Powder metallurgy Method not only reduces experimental risk, simultaneously can be used for producing in enormous quantities, has high prospects for commercial application.

Claims (1)

1. a kind of fabricated in situ nanometer CuAl2/Al2O3The preparation method of reinforced aluminum matrix composites, including the following steps:
(1) mixed-powder is prepared
According to cupric oxide powder: aluminium powder or Al alloy powder mass ratio are to weigh mixed-powder less than 10%.
(2) ball-milling treatment is carried out to mixed-powder
Mixed-powder is fitted into spheroidal graphite tank, ball-milling treatment, ball milling parameter: ratio of grinding media to material are carried out to mixed-powder under protection of argon gas 5:1~15:1, revolving speed 200r/min, Ball-milling Time 1~4 hour.
(3) sinter molding.
CN201810997554.1A 2018-08-29 2018-08-29 A kind of fabricated in situ nanometer CuAl2/Al2O3The preparation method of reinforced aluminum matrix composites Pending CN109082568A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109518033A (en) * 2019-01-18 2019-03-26 福州大学 A kind of situ Al2O3Particle enhanced aluminum-based composite material preparation method
CN110079689A (en) * 2019-05-06 2019-08-02 西南交通大学 A kind of in-situ Al-base composition and preparation method thereof
CN112626367A (en) * 2021-01-06 2021-04-09 山东省科学院新材料研究所 Preparation method of nano alumina particle reinforced aluminum-copper alloy composite material
CN116411199A (en) * 2023-06-12 2023-07-11 内蒙古工业大学 Al 2 O 3 Particles and Al 2 Cu jointly reinforced aluminum-based composite material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1382816A (en) * 2002-05-30 2002-12-04 昆明理工大学 Process for preparing Cu-Al2O3 composition
CN101418396A (en) * 2008-11-25 2009-04-29 陕西科技大学 Method for preparing biphase cooperative strengthening TiAl base composite material
CN107099689A (en) * 2017-05-11 2017-08-29 武汉轻工大学 A kind of Al of reaction in-situ generation2O3The preparation method of particle enhanced aluminum-based composite material
CN108374133A (en) * 2018-03-09 2018-08-07 天津大学 In-situ synthesis of MgAlB4Method for whisker reinforced aluminium base composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1382816A (en) * 2002-05-30 2002-12-04 昆明理工大学 Process for preparing Cu-Al2O3 composition
CN101418396A (en) * 2008-11-25 2009-04-29 陕西科技大学 Method for preparing biphase cooperative strengthening TiAl base composite material
CN107099689A (en) * 2017-05-11 2017-08-29 武汉轻工大学 A kind of Al of reaction in-situ generation2O3The preparation method of particle enhanced aluminum-based composite material
CN108374133A (en) * 2018-03-09 2018-08-07 天津大学 In-situ synthesis of MgAlB4Method for whisker reinforced aluminium base composite material

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109518033A (en) * 2019-01-18 2019-03-26 福州大学 A kind of situ Al2O3Particle enhanced aluminum-based composite material preparation method
CN110079689A (en) * 2019-05-06 2019-08-02 西南交通大学 A kind of in-situ Al-base composition and preparation method thereof
CN110079689B (en) * 2019-05-06 2021-08-03 西南交通大学 In-situ aluminum-based composite material and preparation method thereof
CN112626367A (en) * 2021-01-06 2021-04-09 山东省科学院新材料研究所 Preparation method of nano alumina particle reinforced aluminum-copper alloy composite material
CN112626367B (en) * 2021-01-06 2022-01-11 山东省科学院新材料研究所 Preparation method of nano alumina particle reinforced aluminum-copper alloy composite material
CN116411199A (en) * 2023-06-12 2023-07-11 内蒙古工业大学 Al 2 O 3 Particles and Al 2 Cu jointly reinforced aluminum-based composite material and preparation method thereof
CN116411199B (en) * 2023-06-12 2023-08-04 内蒙古工业大学 Al 2 O 3 Particles and Al 2 Cu jointly reinforced aluminum-based composite material and preparation method thereof

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Application publication date: 20181225