CN106048351A - Preparation method of AIN particle-reinforced magnesium-based composite material - Google Patents
Preparation method of AIN particle-reinforced magnesium-based composite material Download PDFInfo
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- CN106048351A CN106048351A CN201610635178.2A CN201610635178A CN106048351A CN 106048351 A CN106048351 A CN 106048351A CN 201610635178 A CN201610635178 A CN 201610635178A CN 106048351 A CN106048351 A CN 106048351A
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- 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
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1057—Reactive infiltration
- C22C1/1063—Gas reaction, e.g. lanxide
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0068—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 nitrides
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- Materials Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The invention discloses a preparation method of an AIN particle-reinforced magnesium-based composite material and belongs to the technical field of metal-based composite material preparation. The preparation method comprises feeding nitrogen into magnesium alloy melt, simultaneously inserting an ultrasonic probe into the magnesium alloy melt, and preparing the AIN particle-reinforced magnesium-based composite material under control of a reaction temperature, a nitrogen flow, supersonic wave frequency, supersonic wave power and reaction time. The AIN particles produced by the in-situ reaction have small sizes, are dispersed uniformly and have good adhesion to a base interface and a controllable generation amount. The magnesium-based composite material has excellent performances. The preparation method has simple processes, realizes a low cost, can be used for large scale industrial production and has a wide application prospect in the fields of aerospace, automobiles and 3C.
Description
Technical field:
The present invention relates to the preparation method of a kind of AlN particle reinforced magnesium base compound material, particularly under a kind of ultrasonic field
The method of fabricated in situ AlN particle reinforced magnesium base compound material, belongs to metal-base composites preparing technical field.
Background technology:
Along with the development of science and technology, energy-saving and environmental protection become the theme of current era.Many industrial circle such as automobile, aviation, boats
It field is ultralight to exploitation, the demand of the super material of high rigidity, high intensity is increasing, and therefore, particle reinforced Mg-base is combined
Material has been increasingly becoming everybody with advantages such as its high intensity, high rigidity, high elastic modulus and good wearability, creep resistances
The focus of research.
AlN ceramic has the advantages such as high intensity, high rigidity, low-density, low-expansion coefficient, high elastic modulus, high heat conductance,
Lattice parameter is close with magnesium, can be good with the magnesium alloy substrate compatibility as the substrate of the heterogeneous forming core of α-Mg.Using AlN granule as
Particle reinforced magnesium base compound material is prepared in enhancing mutually can make the combination property of magnesium base composite material with Refining Mg Alloy crystal grain simultaneously
Being significantly improved, therefore, AlN is a kind of preferably particulates reinforcements of magnesium base composite material.
The preparation method of AlN particle reinforced magnesium base compound material has stirring casting method, powder metallurgic method, in-situ method etc., example
Such as Chinese patent " preparation method of a kind of thin brilliant Mg based composites containing AlN granule " (CN104928510), by powder smelting
The method that gold is combined with plastic deformation is prepared for high-strength light magnesium base composite material, but this method easily causes particle surface
Pollution, matrix and particle surface wettability are poor, cause the shortcoming such as reduction of boundary strength, and are unfavorable for that large-scale industry is raw
Produce, so there being certain limitation.Ye et al. is by by Mg3N2Powder joins and is prepared for AlN granule reinforced magnesium in AM60B melt
Based composites, but the AlN particle size generated is relatively big and skewness (Materials Letters 58 (2004)
2361-2364).The deficiency of above-mentioned preparation method all will affect the improvement of magnesium base composite material tissue and the raising of combination property.
Summary of the invention:
The technical purpose of the present invention is: for the deficiencies in the prior art, it is provided that prepare AlN granule under a kind of ultrasonic field in situ
The method strengthening magnesium base composite material.The present invention, under the auxiliary of ultrasonic field, utilizes nitrogen to prepare at magnesium alloy fused mass situ
AlN particle reinforced magnesium base compound material, the cavitation of ultrasound wave and acoustic streaming effect, not only can shorten the response time, improve reaction
Productivity, it is also possible to make product evenly, tiny.Method of the present invention possess composite can be mass, technique
Method is easy, granule is uniformly dispersed, strengthen be well combined with basal body interface, environmental friendliness, low cost and other advantages, in aviation boat
My god, the field such as automobile, 3C has broad application prospects.
The present invention is achieved by the following technical solutions, is passed in magnesium alloy fused mass by nitrogen, anti-under ultrasonic field
The time that should set, final cast molding.
The preparation method of AlN particle reinforced magnesium base compound material of the present invention, its step is as follows:
(1) inserting in crucible by a certain amount of magnesium alloy, under the conditions of gas shield, heating and melting is to liquid.
(2) control magnesium alloy fused mass is to design temperature, is passed through in melt by nitrogen, ultrasonic head is inserted magnesium alloy simultaneously and melt
In body, process under nitrogen flow, ultrasonic frequency, ultrasonic power and the response time set.
(3) remove magnesium alloy fused mass top layer scum silica frost, melt is watered and casts from metal pattern or sand mo(u)ld, obtain AlN granule and strengthen
Magnesium base composite material.
Magnesium alloy described in step (1) must contain aluminium element.
Preferred processing condition is as follows:
Described in step (1), in magnesium alloy, the content of aluminium element is 5-30wt.%.
Described in step (2), the purity of nitrogen is not less than 99.99vol%.
Ultrasonic frequency described in step (2) is 20-40kHz, ultrasonic power is 0.2～2kW.
Described in step (2), design temperature is 650～950 DEG C.
Response time described in step (2) is 15～180min.
Nitrogen flow described in step (2) is every 500g magnesium alloy corresponding 15～500ml/min.
Preparation method used by the present invention has the advantage that employing high-energy ultrasonic processes and combines with reaction in-situ, system
Standby go out AlN particle reinforced magnesium base compound material, AlN granule is more tiny and be evenly distributed, AlN granule is good with matrix wettability,
Without interfacial reaction, interface bond strength height, and its growing amount is controlled, the AlN granule reinforced magnesium of final available excellent performance
Based composites, the method is simple, flow process is short and cost is relatively low, can high-volume commercial production, have broad application prospects.
Accompanying drawing illustrates:
Fig. 1 is the preparation technology flow chart that in-situ method prepares AlN particle reinforced magnesium base compound material.
Fig. 2 is the SEM image of AlN particle reinforced magnesium base compound material in embodiment 2.
Fig. 3 is the SEM image of AlN particle reinforced magnesium base compound material in embodiment 4.
Fig. 4 is the TEM image of AlN particle reinforced magnesium base compound material in embodiment 4.
Detailed description of the invention:
The present invention is further illustrated below in conjunction with concrete case study on implementation, it is noted that: following case study on implementation is served only for
The specific implementation method of the bright present invention, can not limit rights protection scope of the present invention.
Embodiment 1:
Present embodiment is prepared the technique of AlN particle reinforced magnesium base compound material and is sequentially included the following steps:
(1) by the magnesium alloy of 500g, (composition is 5.0wt.%Al, 0.85wt.%Zn, 0.01wt.%Mn, 0.01wt.%
Si, surplus are Mg) alloy inserts in crucible, at N2+SF6Under (volume ratio is 1000:1) gaseous mixture protective condition, heating and melting is extremely
Liquid.
(2) control magnesium alloy fused mass is to 650 DEG C, is passed through in melt by nitrogen (purity is 99.99vol.%), simultaneously will be super
Sound head inserts in magnesium alloy fused mass, and ultrasonic frequency is 40kHz.Set nitrogen flow as 500ml/min, ultrasonic power as
2kW, response time are 180min, process under the parameter set.
(3) remove magnesium alloy fused mass top layer scum silica frost, melt is watered and casts from metal pattern or sand mo(u)ld, obtain AlN granule and strengthen
Magnesium base composite material.
Embodiment 2:
Present embodiment is prepared the technique of AlN particle reinforced magnesium base compound material and is sequentially included the following steps:
(1) by the magnesium alloy of 500g, (composition is 9.5wt.%Al, 0.9wt.%Zn, 0.01wt.%Mn, 0.01wt.%
Si, surplus are Mg) alloy inserts in crucible, at CO2+SF6Under (volume ratio is 1000:1) gaseous mixture protective condition, heating and melting is extremely
Liquid.
(2) control magnesium alloy fused mass is to 750 DEG C, is passed through in melt by nitrogen (purity is 99.9999vol.%), will simultaneously
Ultrasonic head inserts in magnesium alloy fused mass, and ultrasonic frequency is 30kHz.Set nitrogen flow as 250ml/min, ultrasonic power as
1kW, response time are 60min, process under the parameter set.
(3) remove magnesium alloy fused mass top layer scum silica frost, melt is watered and casts from metal pattern or sand mo(u)ld, obtain AlN granule and strengthen
Magnesium base composite material.
Embodiment 3:
Present embodiment is prepared the technique of AlN particle reinforced magnesium base compound material and is sequentially included the following steps:
(1) by the magnesium alloy of 500g, (composition is 15.5wt.%Al, 1.2wt.%Zn, 0.02wt.%Mn, 0.02wt.%
Si, surplus are Mg) alloy inserts in crucible, at N2+SF6Under (volume ratio is 1000:3) gaseous mixture protective condition, heating and melting is extremely
Liquid.
(2) control magnesium alloy fused mass is to 950 DEG C, is passed through in melt by nitrogen (purity is 99.999vol.%), will simultaneously
Ultrasonic head inserts in magnesium alloy fused mass, and ultrasonic frequency is 20kHz.Set nitrogen flow as 15ml/min, ultrasonic power as
0.2kW, response time are 15min, process under the parameter set.
(3) remove magnesium alloy fused mass top layer scum silica frost, melt is watered and casts from metal pattern or sand mo(u)ld, obtain AlN granule and strengthen
Magnesium base composite material.
Embodiment 4:
Present embodiment is prepared the technique of AlN particle reinforced magnesium base compound material and is sequentially included the following steps:
(1) by the magnesium alloy of 500g (composition be 30.0wt.%Al, 0.02wt.%Mn, 0.01wt.%Si, surplus are Mg)
Alloy is inserted in crucible, at CO2+SF6Under (volume ratio is 1000:3) gaseous mixture protective condition, heating and melting is to liquid.
(2) control magnesium alloy fused mass is to 800 DEG C, is passed through in melt by nitrogen (purity is 99.9995vol.%), will simultaneously
Ultrasonic head inserts in magnesium alloy fused mass, and ultrasonic frequency is 30kHz.Set nitrogen flow as 150ml/min, ultrasonic power as
0.8kW, response time are 120min, process under the parameter set.
(3) remove magnesium alloy fused mass top layer scum silica frost, melt is watered and casts from metal pattern or sand mo(u)ld, obtain AlN granule and strengthen
Magnesium base composite material.
Although listing the most in detail and illustrating to be preferable to carry out case, but skilled person will appreciate that, can not taking off
Carry out in the case of marrow of the present invention various improvement, add, the mode such as replacement, these contents are all identified as belonging to right and want
Within seeking limited the scope of the present invention.
Claims (8)
1. the preparation method of an AlN particle reinforced magnesium base compound material, it is characterised in that its step includes the following:
(1) inserting in crucible by a certain amount of magnesium alloy, under the conditions of gas shield, heating and melting is to liquid；
(2) control magnesium alloy fused mass is to design temperature, is passed through in melt by nitrogen, ultrasonic head is inserted magnesium alloy fused mass simultaneously
In, process under nitrogen flow, ultrasonic frequency, ultrasonic power and the response time set；
(3) remove magnesium alloy fused mass top layer scum silica frost, melt is watered and casts from metal pattern or sand mo(u)ld, obtain AlN particle reinforced Mg-base
Composite；
Magnesium alloy described in step (1) must contain aluminium element.
2. according to the preparation method of a kind of AlN particle reinforced magnesium base compound material described in claim 1, it is characterised in that step
Suddenly described in (1), in magnesium alloy, the content of aluminium element is 5-30wt.%.
3. according to the preparation method of a kind of AlN particle reinforced magnesium base compound material described in claim 1, it is characterised in that step
Suddenly described in (2), the purity of nitrogen is not less than 99.99vol%.
4. according to the preparation method of a kind of AlN particle reinforced magnesium base compound material described in claim 1, it is characterised in that step
Suddenly ultrasonic frequency described in (2) be 20-40kHz, ultrasonic power be 0.2～2kW.
5. according to the preparation method of a kind of AlN particle reinforced magnesium base compound material described in claim 1, it is characterised in that step
Suddenly design temperature described in (2) is 650～950 DEG C.
6. according to the preparation method of a kind of AlN particle reinforced magnesium base compound material described in claim 1, it is characterised in that step
Suddenly the response time described in (2) is 15～180min.
7. according to the preparation method of a kind of AlN particle reinforced magnesium base compound material described in claim 1, it is characterised in that step
Suddenly nitrogen flow described in (2) is every 500g magnesium alloy corresponding 15～500ml/min.
8. the AlN particle reinforced magnesium base compound material prepared according to claim 1-7 any one method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610635178.2A CN106048351A (en) | 2016-08-04 | 2016-08-04 | Preparation method of AIN particle-reinforced magnesium-based composite material |
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| CN201610635178.2A CN106048351A (en) | 2016-08-04 | 2016-08-04 | Preparation method of AIN particle-reinforced magnesium-based composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834848A (en) * | 2017-01-18 | 2017-06-13 | 北京工业大学 | A kind of in-situ particle reinforced magnesium-based composite material and preparation method thereof |
| EP3896182A1 (en) * | 2020-04-16 | 2021-10-20 | Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung GmbH | Magnesium alloy, in particular for laser build-up welding |
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|---|---|---|---|---|
| CN101381829A (en) * | 2008-10-17 | 2009-03-11 | 江苏大学 | Method for preparing in-situ particle reinforced magnesium base compound material |
| CN101608277A (en) * | 2009-06-02 | 2009-12-23 | 大连理工大学 | A kind of electromagnetic/ultrasonic preparation method of in-situ particle reinforced magnesium-based composite material |
| CN104313371A (en) * | 2014-09-29 | 2015-01-28 | 南昌大学 | Method for preparing magnesium matrix composite semisolid slurry by adopting ultrasonic in situ synthesis |
| CN105463232A (en) * | 2015-12-04 | 2016-04-06 | 西北工业大学 | Preparing method for high-strength and high-plasticity AlN/AZ91D magnesium matrix composite |
| CN105695770A (en) * | 2016-01-28 | 2016-06-22 | 大连理工大学 | Method for in-situ preparation of Al2X particle reinforced magnesium base composite material |
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2016
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381829A (en) * | 2008-10-17 | 2009-03-11 | 江苏大学 | Method for preparing in-situ particle reinforced magnesium base compound material |
| CN101608277A (en) * | 2009-06-02 | 2009-12-23 | 大连理工大学 | A kind of electromagnetic/ultrasonic preparation method of in-situ particle reinforced magnesium-based composite material |
| CN104313371A (en) * | 2014-09-29 | 2015-01-28 | 南昌大学 | Method for preparing magnesium matrix composite semisolid slurry by adopting ultrasonic in situ synthesis |
| CN105463232A (en) * | 2015-12-04 | 2016-04-06 | 西北工业大学 | Preparing method for high-strength and high-plasticity AlN/AZ91D magnesium matrix composite |
| CN105695770A (en) * | 2016-01-28 | 2016-06-22 | 大连理工大学 | Method for in-situ preparation of Al2X particle reinforced magnesium base composite material |
Non-Patent Citations (2)
| Title |
|---|
| H.Z. YE ET AL.: ""In situ synthesis of AlN in Mg-Al alloys by liquid nitridation"", 《JOURNAL OF MATERIALS PROCESSING TECHNOLOGY》 * |
| 张文清 主编: "《分离分析化学》", 31 July 2016 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834848A (en) * | 2017-01-18 | 2017-06-13 | 北京工业大学 | A kind of in-situ particle reinforced magnesium-based composite material and preparation method thereof |
| CN106834848B (en) * | 2017-01-18 | 2018-06-01 | 北京工业大学 | A kind of in-situ particle reinforced magnesium-based composite material and preparation method thereof |
| EP3896182A1 (en) * | 2020-04-16 | 2021-10-20 | Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung GmbH | Magnesium alloy, in particular for laser build-up welding |
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