CN105506341A - Mg alloy/Al2O3 composite and preparation method thereof - Google Patents

Mg alloy/Al2O3 composite and preparation method thereof Download PDF

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CN105506341A
CN105506341A CN201610117509.3A CN201610117509A CN105506341A CN 105506341 A CN105506341 A CN 105506341A CN 201610117509 A CN201610117509 A CN 201610117509A CN 105506341 A CN105506341 A CN 105506341A
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alloy
matrix
matrix material
preparation
laminate structure
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CN105506341B (en
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沈平
刘艳
郭瑞芬
张恒
阿拉腾沙嘎
付玉洁
姜启川
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Jilin University
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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
    • 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
    • C22C1/1005—Pretreatment of the non-metallic additives
    • C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
    • 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
    • C22C1/1005—Pretreatment of the non-metallic additives
    • C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
    • C22C1/1021—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform the preform being ceramic
    • 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
    • C22C1/1057—Reactive infiltration
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • 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
    • C22C32/001—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 only oxides
    • C22C32/0015—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 only oxides with only single oxides as main non-metallic constituents
    • C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

The invention relates to an Mg alloy/Al2O3 composite light in weight and high in strength, in particular to an Mg alloy/Al2O3 composite and a preparation method thereof. The Mg alloy/Al2O3 composite is composed of a lamellar structure Al2O3 substrate prepared by an ice template method and Mg alloy composited in lamellar spacing of the substrate by impregnation, and is obtained by soaking in a silica sol a lamellar structure Al2O3 base made by ice template oriented solidification so that nano SiO2 covers the surface of Al2O3 lamellas, and carrying Mg alloy impregnation in Ar atmosphere. This composite has high specific strength and has compressive strength up to 697 MPa when its density is 2.57 g/cm<3>.

Description

Mg alloy/Al 2o 3matrix material and preparation method
Technical field
The present invention relates to the metal/ceramic composite of high-strength light, particularly a kind of Mg alloy/Al 2o 3matrix material and preparation method thereof.
Background technology
Along with the development of science and technology, the high-strength lightization of material certainly will become the development trend in the fields such as aerospace, automotive industry and bulletproof armour.And Mg alloy is minimum at metallic substance Midst density, be about 2/3 of Al alloy, thus become the first-selection of lightweight structural material.But Mg alloy strength is low, thus need to increase its intensity by methods such as compounds.Stupalith intensity is high, but plasticity is poor.The structured material both compounds being obtained high-strength light can meet application demand.But how effectively compound is the key factor determining Mg alloy/ceramic composite performance.
20 century 70s, it is found that the microtexture that natural seashell has " brick-mud ", and its composition is crystalline calcium carbonate and albumen organism.Organic content is only about 5vol.%, and inorganic carbonate calcium layer is interconnected by organic " glue ", and distribute in laminate structure, thickness is approximately 0.3 – 0.4 μm.The work of rupture of this laminate structure is than simple calcium carbonate height about 3000 times.Based on the good characteristic of concba lamellar structure, people start to seek the layer structure material how preparing imitative shell.It is found that by freezing to the orientation of water based suspension, ice crystal and solute can be made to be layered distribution, then distilled by ice crystal through vacuum lyophilization, thus obtain the laminate structure of solute, this i.e. ice template method.The standby imitative shell stratiform porous ceramic film material of ice template legal system is utilized both to overcome the shortcoming that traditional production technique (as flow casting molding, reaction sintering etc.) cannot realize microtexture precise controlling (thickness in monolayer is less than 100 μm), overcome layer-layer to pile up, self-assembly etc. cannot prepare the shortcoming of big scale structural timber simultaneously.
In recent years, the standby imitative shell stratiform porous ceramic film material of ice template legal system is utilized to become study hotspot.But this method combined with metallic infiltration technology, be injected in layered porous ceramic hole prepared by ice template by metal melt, the research obtaining laminated metal-ceramic composite is also little.At present, we can retrieve only several sections of documents (Minimalcompliancedesignformetal – ceramiccompositeswithlamellarmicrostructures, ActaMater, 59 volume P4835 – 4846 in 2011 in the world; Lamellar – interpenetratedAl – Si – Mg/SiCcompositesfabricatedbyfreezecastingandpressureless infiltration, Mater.Sci.Eng.A, 630 volume P78 – 84 in 2015; Preparationofhigh – strengthAl – Mg – Si/Al 2o 3compositeswithlamellarstructuresusingfreezecastingandpre ssurelessinfiltrationtechniques, ActaMetall.Sin., 27 volume 5 phase P944 – 950 in 2014) concentrate on Al based composites, infiltration process is Pressure Infiltration and pressure-free impregnation two kinds mainly.Do not retrieve any report about utilizing ice template and infiltration technique to prepare Mg based composites.In the preparation of stratiform Al based composites, the bearing requirements of Pressure Infiltration to equipment and ceramic body is higher, and need the high pressure resistant mould of high-tension apparatus and good seal, so production cost is high, technique is more complicated.And pressure-free impregnation utilizes capillary force effect to penetrate in the layered poros of porous ceramics by spontaneous for molten alloy, low to the bearing requirements of equipment and ceramic body, cost is low, and technique is simple.But the maximum bottleneck of pressure-free impregnation is the Problem of Wettability that will solve metal and ceramic body.That is, only have on the basis of good wet at both, molten alloy spontaneous infiltration just can be made to enter porous ceramics base substrate.Previously, China Patent Publication No. CN201410072030.3, publication date on July 2nd, 2014, denomination of invention is high strength stratiform Al based ceramic metal matrix material and preparation method thereof, discloses a kind of high strength stratiform Al based ceramic metal matrix material and preparation method thereof.Mainly make use of Mg and N in Al alloy in the process 2gas changes Al 2o 3wettability between pottery and Al alloy, thus realize pressure-free impregnation.The ultimate principle of this method is at N 2under atmosphere, by Al-Si-Mg alloy heating and melting, utilize the Mg in Al alloy (mass ratio of Mg is 6-10wt.%) to evaporate and become Mg steam, with N 2reaction generates Mg 3n 2.Mg 3n 2be attached to Al 2o 3on lamella, continue to react generating AlN and displacing Mg with the Al in aluminium alloy forward position.The AlN generated significantly reduces the interfacial energy of liquid-solid interface, improves the wettability between alloy and pottery, thus realizes the pressure-free impregnation of Al-Si-Mg alloy in ceramic layered base substrate.In the pressure-free impregnation of Al-Si-Mg alloy, Mg and N of certain content 2atmosphere is two prerequisites.But for Mg alloy, due to Mg and N 2large quantitative response can generate Mg 3n 2phase, cause alloy pulverization serious, and fragility is large, so should not adopt nitrogen containing atmosphere, thus also cannot realize metal and ceramic soaking.That is, above-mentioned pressure-free impregnation can not for the preparation of Mg Base Metal-ceramic laminar composite material.
Summary of the invention
The object of the invention is to propose a kind of Mg alloy/Al 2o 3matrix material and preparation method, realize obtaining the high Mg alloy/Al of specific tenacity with the technology of preparing of low cost 2o 3matrix material.
Mg alloy/Al of the present invention 2o 3matrix material is by the standby laminate structure Al of ice template legal system 2o 3matrix and the Mg alloy composition be compounded in this base sheet lamellar spacing that infiltrates.
The preferred structure of this matrix material is: Mg alloy layer and Al 2o 3the thickness of layer is 25 – 100 μm; Al 2o 3volume fraction be 10 – 40vol.%, the volume fraction of Mg alloy is 60 – 90vol.%.
Mg alloy/Al of the present invention 2o 3the preparation method of matrix material, comprises the following steps:
A. the Al of laminate structure is obtained by ice template method directional freeze 2o 3base substrate, and at high temperature sintering obtains laminate structure Al 2o 3matrix;
B. by above-mentioned Al 2o 3after matrix soaks in silicon sol, be dried at 700 – 950 DEG C and dewater completely; Make Nano-meter SiO_2 2be coated on Al 2o 3sheet surfaces;
C. Mg alloy block is placed in the Al after step b process 2o 3on matrix, put into retort furnace, heat up with stove under an ar atmosphere, infiltrate at 630-700 DEG C, cool to room temperature with the furnace, namely obtain Mg alloy layer and Al 2o 3layer is in alternatively distributed Mg alloy/Al 2o 3matrix material.
Laminate structure Al described in step a 2o 3matrix, is obtained by following embodiment:
By Al 2o 3the aqueous solution of powder containing Disperser Polysodium Methacrylate, wherein Al 2o 3the volume percent that powder accounts for whole slurry is 10-40vol.%, at grinding in ball grinder final vacuum stirring degassing, and the water base Al that obtained particle diameter is less than 5 μm 2o 3slurry;
By water base Al 2o 3slurry injects Teflon mould, after carrying out directional freeze, carries out vacuum-sublimation dehydration, then sinters at 1300-1500 DEG C, obtain the laminate structure Al with directed porosity under freeze drier Zhong – 50 DEG C and 10Pa in the low temperature bath of-20 DEG C 2o 3matrix.
Silicon sol described in step b, SiO 2concentration is 10-30wt.%, SiO 2particle diameter is 10 – 20nm, and soak time is 2 – 120min.
Intensification described in step c and speed of cooling are 5 DEG C/min, and described Mg alloy can be selected from the various commercial trade mark, and wherein in typical AZ series magnesium alloy, the content of magnesium is 90-100wt.%, and the content of aluminium is 1-10wt.%, and the content of zinc is 0.35-1wt.%.
Mg alloy/Al provided by the invention 2o 3matrix material, has expanded high-strength light metal-ceramic composite material kind further.When the density of this matrix material is 2.57g/cm 3time, its compressive strength can reach 697MPa.
Due to Mg alloy and Al 2o 3the wettability of pottery is poor, cannot enter porous Al by spontaneous infiltration after Mg alloy melting 2o 3in base substrate.Therefore, in preparation method, the present invention proposes silicon sol infusion method and reaction spontaneous infiltration technology.Silicon sol infusion method easily can realize Nano-meter SiO_2 2coated Al 2o 3pottery sheet surfaces, thus significantly improve the wettability with Mg alloy; And react spontaneous infiltration compared to traditional Pressure Infiltration and pressure-free impregnation, have equipment simple, technique is simple, and low to the bearing requirements of ceramic body, cost is low, and infiltration speed is fast, and alloy fillibility is good, and interface cohesion is not by force and by N 2the advantages such as atmosphere restriction.
Accompanying drawing explanation
Fig. 1 is the Al that the embodiment of the present invention 4 ice template method directional freeze obtains laminate structure 2o 3base substrate, along the vertical section scanning electron photomicrograph being parallel to ice-crystal growth direction;
Fig. 2 is the Al that the embodiment of the present invention 4 obtains 2o 3matrix soaks silicon sol, dried vertical section scanning electron photomicrograph;
Fig. 3 is the stress under compression-strain curve figure of the matrix material of the embodiment of the present invention 1,2,3,4;
Matrix material upper part vertical section optical microscope photograph prepared by Fig. 4 embodiment of the present invention 4.
Embodiment
Below by way of the embodiment enumerated, the present invention is further elaborated.
Mg alloy/Al of the present invention 2o 3the preparation of matrix material:
1. water base Al 2o 3the preparation of slurry
Disperser Polysodium Methacrylate is dissolved in the aqueous solution of 40 DEG C, then and Al 2o 3powder mixes, and adopts rotating speed to be that the planetary ball mill ball milling 6h of 100r/min makes ceramic size, wherein Al 2o 3the volume percent that powder accounts for whole slurry is 10-40vol.%, and dispersant is Al 2o 3the 1wt.% of powder, by the slurry vacuum stirring degasification 20min after ball milling, stirring velocity is 80-100r/min, the water base Al that obtained particle diameter is less than 5 μm 2o 3slurry.
2. directional freeze
Above-mentioned water base Al 2o 3slurry inject Teflon mould ,-20 DEG C low temperature bath in carry out directional freeze, water freeze process in, Al 2o 3particle squeezes in the gap of ice crystal, forms oriented laminated arrangement, obtains the stratiform Al with directional profile 2o 3cylinder shape base substrate, blank diameter is 18-30mm, is highly about 25-30mm.
3. lyophilize
By above-mentioned Al 2o 3put into freeze drier rapidly after the base substrate demoulding, the distillation carrying out ice crystal under vacuum state is removed, and freezing temp is-50 DEG C, and vacuum tightness is 10Pa, and time of drying is 24h.
4. the sintering of base substrate
Dried Al 2o 3base substrate carries out high temperature sintering in atmosphere, namely obtains the laminate structure Al with directed porosity 2o 3matrix; Sintering process parameter is: 0-300 DEG C of heat-up rate is 4 DEG C/min, and being incubated 30min, 300-900 DEG C of heat-up rate when 300 DEG C is 5 DEG C/min, is incubated 30min, then continues to be raised to 1300-1500 DEG C with 5 DEG C/min when 900 DEG C, insulation 2h.
5. soak silicon sol
By above-mentioned Al 2o 3matrix is immersed in SiO 2concentration is 10-30wt.%, SiO 2particle diameter is in the silicon sol of 10 – 20nm, soaks 2-120min.
6. dry
By the above-mentioned Al through soaking silicon sol 2o 3matrix is dried to and dewaters completely at 700 – 950 DEG C; Make Nano-meter SiO_2 2be coated on Al 2o 3matrix sheet surfaces;
7. infiltrate
Mg alloy block is placed in the Al after above-mentioned process 2o 3on matrix, put into tube furnace together, prepurging in advance (is evacuated to below 2Pa, then passes into high-purity Ar gas for 2 times, circulate twice), under an ar atmosphere, be warming up to 630-700 DEG C with 5 DEG C/min, insulation 10min, then 5 DEG C/min is cooled to room temperature, is infiltrated up to Al completely by Mg alloy 2o 3in the layered poros of matrix, finally obtain Mg alloy and Al 2o 3in the laminate structure Mg alloy/Al replacing lamella arrangements 2o 3matrix material.
The Mg alloy used that infiltrates can be selected from the various commercial trade mark, and wherein in typical AZ series magnesium alloy, the content of magnesium is 90-100wt.%, and the content of aluminium is 1-10wt.%, and the content of zinc is 0.35-1wt.%.
By adjusting water base Al 2o 3the Al of slurry 2o 3the volume percent of whole slurry shared by powder, can obtain the described Al with different aperture degree 2o 3matrix, that is determine the final Mg alloy/Al obtained 2o 3al in matrix material 2o 3with the volume ratio of Mg alloy;
By regulating concentration and the soak time of silicon sol, can control Al 2o 3siO in matrix lamella 2content, and then control the cracking phenomena of infiltration speed and matrix material;
Table 1 is Mg alloy/Al prepared under various processing parameter below 2o 3the embodiment of matrix material.
Table 1
The embodiment of the present invention 4 ice template method directional freeze obtains the Al of laminate structure 2o 3base substrate, is shown in shown in accompanying drawing 1 along the vertical section scanning electron photomicrograph being parallel to ice-crystal growth direction.
The Al that the embodiment of the present invention 4 is obtained 2o 3matrix soaks silicon sol, dried vertical section scanning electron photomicrograph is shown in shown in accompanying drawing 2; Wherein macrobead is A1 2o 3, small-particle is SiO 2, Nano-meter SiO_2 2there is agglomeration.
Matrix material upper part vertical section optical microscope photograph prepared by the embodiment of the present invention 4 is shown in shown in accompanying drawing 4; Wherein white is metal level, and black is A1 2o 3ceramic layer.
Fig. 3 is the stress under compression-strain curve figure of the matrix material of listed embodiment 1,2,3,4 in table 1, can learn along with Al 2o 3the increase of volume fraction, the intensity of matrix material increases.

Claims (6)

1. Mg alloy/Al 2o 3matrix material, is characterized in that, is by the standby laminate structure Al of ice template legal system 2o 3matrix and the Mg alloy composition be compounded in this base layer gap that infiltrates.
2. Mg alloy/Al according to claim 1 2o 3matrix material, is characterized in that, its Mg alloy layer and Al 2o 3the thickness of layer is 25 – 100 μm; Al 2o 3volume fraction be 10 – 40vol.%, the volume fraction of Mg alloy is 60 – 90vol.%.
3. Mg alloy/Al according to claim 1 2o 3the preparation method of matrix material, is characterized in that comprising the following steps:
A. the Al of laminate structure is obtained by ice template method directional freeze 2o 3base substrate, and at high temperature sintering obtains laminate structure Al 2o 3matrix;
B. by above-mentioned Al 2o 3after matrix soaks in silicon sol, be dried at 700 – 950 DEG C and dewater completely;
C. Mg alloy block is placed in the Al after step b process 2o 3on matrix, put into retort furnace, heat up with stove under an ar atmosphere, infiltrate at 630-700 DEG C, cool to room temperature with the furnace, namely obtain Mg alloy layer and Al 2o 3layer is in alternatively distributed Mg alloy/Al 2o 3matrix material.
4. Mg alloy/Al according to claim 3 2o 3the preparation method of matrix material, is characterized in that, the laminate structure Al described in step a 2o 3matrix, is obtained by following embodiment:
By Al 2o 3the aqueous solution of powder containing Disperser Polysodium Methacrylate, wherein Al 2o 3the volume percent that powder accounts for whole slurry is 10-40vol.%, at grinding in ball grinder final vacuum stirring degassing, and the water base Al that obtained particle diameter is less than 5 μm 2o 3slurry;
By water base Al 2o 3slurry injects Teflon mould, after carrying out directional freeze, carries out vacuum-sublimation dehydration, then sinters at 1300-1500 DEG C, obtain the laminate structure Al with directed porosity under freeze drier Zhong – 50 DEG C and 10Pa in the low temperature bath of-20 DEG C 2o 3matrix.
5. Mg alloy/Al according to claim 3 2o 3the preparation method of matrix material, is characterized in that, the silicon sol described in step b, SiO 2concentration is 10-30wt.%, SiO 2particle diameter is 10 – 20nm, and soak time is 2 – 120min.
6. Mg alloy/Al according to claim 3 2o 3the preparation method of matrix material, is characterized in that, the intensification described in step c and speed of cooling are 5 DEG C/min, and described Mg alloy can be selected from the various commercial trade mark.
CN201610117509.3A 2016-03-02 2016-03-02 Mg alloys/Al2O3Composite material and preparation method Expired - Fee Related CN105506341B (en)

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Cited By (7)

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CN107522475A (en) * 2017-09-08 2017-12-29 大连理工大学 A kind of imitative shell ceramic matric composite and preparation method thereof
CN107746985A (en) * 2017-10-09 2018-03-02 常州禾吉纺织品有限公司 A kind of preparation method of stratiform interworking architecture composite
CN113277851A (en) * 2021-06-29 2021-08-20 中国科学院金属研究所 Ceramic-metal bionic nano composite material and preparation method thereof
CN113560542A (en) * 2021-07-15 2021-10-29 北京交通大学 Dual-continuous-phase Ti with controllable reinforced phase2AlN/Mg-based composite material and pressureless infiltration preparation method thereof
CN114058920A (en) * 2021-11-22 2022-02-18 吉林大学 Shell brick mud structure-imitated high-volume ceramic-metal composite material and preparation method thereof
CN116536538A (en) * 2023-07-05 2023-08-04 太原理工大学 Preparation method of ultrasonic-assisted self-infiltration aluminum oxide reinforced magnesium-based composite material
CN117845093A (en) * 2024-03-07 2024-04-09 太原理工大学 Preparation method of SiC/AZ91 composite material impregnated by vacuum air pressure

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107522475A (en) * 2017-09-08 2017-12-29 大连理工大学 A kind of imitative shell ceramic matric composite and preparation method thereof
CN107522475B (en) * 2017-09-08 2019-12-27 大连理工大学 Shell-like ceramic matrix composite and preparation method thereof
CN107746985A (en) * 2017-10-09 2018-03-02 常州禾吉纺织品有限公司 A kind of preparation method of stratiform interworking architecture composite
CN113277851A (en) * 2021-06-29 2021-08-20 中国科学院金属研究所 Ceramic-metal bionic nano composite material and preparation method thereof
CN113277851B (en) * 2021-06-29 2022-05-24 中国科学院金属研究所 Ceramic-metal bionic nano composite material and preparation method thereof
CN113560542A (en) * 2021-07-15 2021-10-29 北京交通大学 Dual-continuous-phase Ti with controllable reinforced phase2AlN/Mg-based composite material and pressureless infiltration preparation method thereof
CN114058920A (en) * 2021-11-22 2022-02-18 吉林大学 Shell brick mud structure-imitated high-volume ceramic-metal composite material and preparation method thereof
CN116536538A (en) * 2023-07-05 2023-08-04 太原理工大学 Preparation method of ultrasonic-assisted self-infiltration aluminum oxide reinforced magnesium-based composite material
CN116536538B (en) * 2023-07-05 2023-09-08 太原理工大学 Preparation method of ultrasonic-assisted self-infiltration aluminum oxide reinforced magnesium-based composite material
CN117845093A (en) * 2024-03-07 2024-04-09 太原理工大学 Preparation method of SiC/AZ91 composite material impregnated by vacuum air pressure
CN117845093B (en) * 2024-03-07 2024-05-03 太原理工大学 Preparation method of SiC/AZ91 composite material impregnated by vacuum air pressure

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