CN101148722A - In situ self-generation aluminum nitride and magnesium disilicide enhanced magnesium-base composite material and preparation method thereof - Google Patents
In situ self-generation aluminum nitride and magnesium disilicide enhanced magnesium-base composite material and preparation method thereof Download PDFInfo
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- CN101148722A CN101148722A CNA2007100479444A CN200710047944A CN101148722A CN 101148722 A CN101148722 A CN 101148722A CN A2007100479444 A CNA2007100479444 A CN A2007100479444A CN 200710047944 A CN200710047944 A CN 200710047944A CN 101148722 A CN101148722 A CN 101148722A
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- silicon
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Abstract
The Mg-base composite material with in-situ autogeneous reinforcing AlN and Mg2Si phases contains Mg alloy base in 64-97.6 wt% and reinforcing AlN and Mg2Si ceramic phases in 2.4-36 wt%. Its Mg alloy base contains Al in 0-9 wt% and Mg for the rest, and the reinforcing phases include AlN in 1-15 wt% and Mg2Si in 1.4-21 wt%. The Mg-base composite material is prepared through the following steps: 1. melting Mg-Al alloy material under the protection of mixed SF6+CO2 gas; 2. pressing aluminum foil coated Si3N4 powder into the Mg-Al melt; 3. further heating and maintaining; and 4. cooling, maintaining, stirring the melt and skimming the scum with a graphite disc, casting into metal mold and solidifying to obtain the composite material. The composite material has the features of light weight, high strength, high modulus, high heat resistance, etc.
Description
Technical field
The present invention relates to a kind of technical field of composite materials magnesium base composite material and preparation method thereof, particularly a kind of in-situ authigenic aluminium nitride and magnesium two silicon strengthen magnesium base composite material and preparation method thereof.
Background technology
Magnesium alloy is the lightest structural metallic materials in the present industrial application, have higher specific tenacity, specific rigidity and good casting, damping, machining, performance such as electromagnetic shielding and reusable edible makes it extensively be used to 3C Product, in aircraft industry and the automotive industry.The raising that requires along with energy-saving consumption-reducing in the communications and transportation and to the pay attention to day by day of environmental protection impels magnesium alloy application potential in this respect more; But the performance requriements to magnesium alloy is also more and more higher simultaneously, and ordinary magnesium alloy can not satisfy these requirements, and people begin to develop the magnesium base composite material with comprehensive high-performance.
Find through literature search prior art, people such as Hai Zhi Ye, at " Journal of MaterialsScience " (Materials science journal, 39 (2004): 2153-2171), write articles " Review of recent studieson magnesium matrix composites (magnesium base composite material progress) ".This article is summarized method of preparing magnesium-based composite material, and wherein major part is to adopt to add legal system and be equipped with particle reinforced magnesium base compound material; Adding legal system is equipped with magnesium base composite material and has many shortcomings: (1) is because the general special equipment of needs of outer adding method has increased manufacturing cost; (2) because ceramic particle and matrix metal are nonwetting, be difficult to prepare the equally distributed metal-base composites of ceramic particle; (3) it is certain to add the ceramic particle size, has limited the size of wild phase; (4) ceramic particle combines badly with the interface of metal, has influence on its final properties; (5) bad surface reaction takes place in ceramic particle and metal melt, has influence on its final properties.In this piece document, also mentioned the method for some in-situ preparing magnesium base composite materials.But, the wild phase that the reaction in that does not still find at present generates mutually, at present main is that original position forms Mg
2The Si monophased particles strengthens; And because Mg
2The performance that Si is not high, as Young's modulus 120GPa only, it is very limited that the performance of gained magnesium base composite material improves.
Summary of the invention
The present invention is directed to the defective in the background technology, provide a kind of in-situ authigenic aluminium nitride and magnesium two silicon to strengthen magnesium base composite material and preparation method thereof,, prepare a kind of at the inner self-generating (AlN+Mg of magnesium alloy by stirring casting method and in-situ reaction are combined
2Si) multiphase ceramic particle reinforced magnesium base compound material makes it satisfy the needs of lightweight, high-strength, high elastic coefficient, resistance to elevated temperatures.
The present invention is achieved by the following technical solutions:
In-situ authigenic aluminium nitride involved in the present invention and magnesium two silicon enhancing magnesium base composite material are by magnesium alloy substrate and contain AlN and Mg simultaneously
2Si two ceramic phase particles constitute jointly, and the weight percent content of magnesium alloy substrate is 64%-97.6%, contains AlN and Mg simultaneously
2Si two ceramic phase particle weight percent contents are 2.4%--36%.
In the described magnesium alloy substrate, the aluminium weight percent content is 0%--9%, and surplus is Mg.
Described AlN and the Mg of containing simultaneously
2In Si two ceramic phase particles, the degree that the AlN particle accounts for the magnesium base composite material gross weight is 1%--15%, Mg
2The degree that the Si particle accounts for the magnesium base composite material gross weight is 1.4-21%.
In-situ authigenic aluminium nitride involved in the present invention and magnesium two silicon strengthen method of preparing magnesium-based composite material, may further comprise the steps:
(1) at SF
6And CO
2Under the mixed gas protected condition, the magnalium starting material are melted fully;
(2) then the Si that wraps with aluminium foil
3N
4Powder is pressed in the magnalium melt;
(3) in melt, add Mg
3N
2Behind the powder, heat up and insulation, to guarantee Si
3N
4Mg in powder and the magnalium melt, Al complete reaction;
(4) back cooling and insulation are finished in insulation, and after stirring melt with graphite disk, drag for the scum silica frost on surface, and water to cast from and obtain in-situ authigenic aluminium nitride of the present invention and magnesium two silicon enhancing magnesium base composite material after metal die solidifies.
In the step (1), described fusing, its temperature is controlled between 680-720 ℃.
In the step (1), described SF
6And CO
2Mixed gas, wherein SF
6Volume accounts for 10%, CO
2Volume accounts for 90%.
In the step (2), described Si
3N
4Powder, its particle size are 0.5 μ m-45 μ m.
In the step (3), described intensification, its temperature rises to 800 ℃-900 ℃.
In the step (3), described insulation, its time is 30 minutes-90 minutes;
In the step (4), the described temperature that is cooled to is 680 ℃-720 ℃, and stirring velocity is 200-1000r/min, and churning time is 10 minutes-40 minutes.
The present invention is with magnalium and Si
3N
4Powder is starting material, according to 4[Al]
In Mg alloy+ 6[Mg]+Si
3N
4(s)=4AlN (s)+3Mg
2Si (s), i.e. 4molAl and 6molMg and 1mol Si in the magnalium melt
3N
4Reaction generates 4molAlN and 3molMg
2Si guarantees Si
3N
4Form AlN and Mg with Mg, Al complete reaction in the magnalium melt
2Si two ceramic phase particles, and the preparation method who adopts stirring casting method and in-situ reaction to combine.Because AlN and Mg
2The Si ceramic particle in the stirring casting process by chemical reaction self-generating in magnesium alloy substrate, good with the interface compatibility of matrix, the particle size of wild phase is controlled, wild phase characteristics such as be evenly distributed, thereby the magnesium base composite material of preparation has favorable mechanical and physicals; And avoided tradition to add legal system when being equipped with matrix material, problems such as size-constrained system, wild phase and the matrix bond of wild phase is bad, wild phase skewness effectively.
The present invention is simple and direct under the condition that does not change original stirring casting equipment and technical process, prepares the original position magnesium base composite material at low cost; And the AlN ceramic phase Young's modulus of the inner self-generating of magnesium alloy is 310GPa, and its reinforced effects is much better than single Mg
2Si strengthens, and can significantly improve the Young's modulus of matrix material; And the AlN ceramic phase of self-generating to have a crystalline structure of close-packed hexagonal structure (lattice parameter is a:0.3113nm c:0.4981nm) and magnesium identical and lattice parameter (a:0.3202nm c:0.5199nm) is close, form good interface structure (as coherence or semicoherent interface) easily, thereby can prepare the superior magnesium base composite material of physical and mechanical property.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment one:
At 10vol.%SF
6+ 90vol.%CO
2Under the mixed gas protected condition, pure magnesium ingot (98.4wt.%) and fine aluminium ingot (0.7wt.%) are melted fully at 680 ℃, then the Si that wraps with aluminium foil
3N
4(0.9wt.%) powder is pressed in the melt, Si
3N
4Particle size is 0.5 μ m.Then temperature is elevated to 800 ℃, and continues insulation 90 minutes, guarantee Si
3N
4Mg in powder and the melt, Al complete reaction cool to 680 ℃ of insulations after insulation is finished, and stir melt with the graphite disk stirring arm, and stirring velocity is 1000r/min, and churning time is 10 minutes.Drag at last to water to cast from behind the scum silica frost on surface and obtain 2.4wt.% (AlN+Mg after solidifying in the metal die
2Si)/and pure Mg matrix material, wherein the weight fraction of AlN is 1%, Mg
2The weight fraction of Si is 1.4%.Gained (AlN+Mg
2Si) density of the pure magnesium base composite material of enhancing is: 1.75g/cm
3, Young's modulus is: 47GPa, tensile property is: 230MPa, 150 ℃ of tensile strengths are: 200MPa.
Embodiment two:
At 10vol.%SF
6+ 90vol.%CO
2Under the mixed gas protected condition, pure magnesium ingot (81.1wt.%) and fine aluminium ingot (10.4wt.%) are melted fully at 700 ℃, then the Si that wraps with aluminium foil
3N
4(8.5wt.%) powder is pressed in the melt, Si
3N
4Particle size is 1 μ m.Then temperature is elevated to 850 ℃, and continues insulation 60 minutes, guarantee Si
3N
4Mg in powder and the melt, Al complete reaction cool to 700 ℃ of insulations after insulation is finished, and stir melt with the graphite disk stirring arm, and stirring velocity is 600r/min, and churning time is 20 minutes.Drag at last to water to cast from behind the scum silica frost on surface and obtain 24wt.% (AlN+Mg after solidifying in the metal die
2Si)/and the Mg-5wt.% matrix material, wherein the weight fraction of AlN is 10%, Mg
2The weight fraction of Si is 14%.Gained (AlN+Mg
2Si) strengthen that to contain the aluminium weight fraction be that the density of 5% magnalium based composites is 1.85g/cm
3, Young's modulus is: 70GPa, tensile property is: 310MPa, 150 ℃ tensile strength is 280MPa.
Embodiment three:
At 10vol.%SF
6+ 90vol.%CO
2Under the mixed gas protected condition, pure magnesium ingot (71.5wt.%) and fine aluminium ingot (15.7wt.%) are melted fully at 720 ℃, then the Si that wraps with aluminium foil
3N
4(12.8wt.%) powder is pressed in the melt, Si
3N
4Particle size is 40 μ m.Then temperature is elevated to 900 ℃, and continues insulation 30 minutes, guarantee Si
3N
4Mg in powder and the melt, Al complete reaction cool to 720 ℃ of insulations after insulation is finished, and stir melt with the graphite disk stirring arm, and stirring velocity is 200r/min, and churning time is 40 minutes.Drag at last to water to cast from behind the scum silica frost on surface and obtain 36wt.% (AlN+Mg after solidifying in the metal die
2Si)/and the Mg-9wt.%Al matrix material, wherein the weight fraction of AlN is 15%, Mg
2The weight fraction of Si is 21%.Gained (AlN+Mg
2Si) strengthen that to contain the aluminium weight fraction be that the density of 9% magnalium based composites is: 1.91g/cm
3, Young's modulus is: 84GPa, tensile property is: 350MPa, 150 ℃ of tensile strengths are: 320MPa.
Claims (10)
1. in-situ authigenic aluminium nitride and magnesium two silicon strengthen magnesium base composite material, it is characterized in that, are by magnesium alloy substrate and contain AlN and Mg simultaneously
2Si two ceramic phase particles constitute jointly, and wherein: the weight percent content of magnesium alloy substrate is: 64%-97.6%, contain AlN and Mg simultaneously
2Si two ceramic phase particle weight percent contents are: 2.4%--36%.
2. in-situ authigenic aluminium nitride according to claim 1 and magnesium two silicon strengthen magnesium base composite material, and it is characterized in that in the described magnesium alloy substrate, the aluminium weight percent content is: 0%--9%, surplus is Mg.
3. in-situ authigenic aluminium nitride according to claim 1 and magnesium two silicon strengthen magnesium base composite material, it is characterized in that described AlN and the Mg of containing simultaneously
2In Si two ceramic phase particles, the degree that the AlN particle accounts for the magnesium base composite material gross weight is 1%--15%, Mg
2The degree that the Si particle accounts for the magnesium base composite material gross weight is 1.4-21%.
4. in-situ authigenic aluminium nitride as claimed in claim 1 and magnesium two silicon strengthen method of preparing magnesium-based composite material, it is characterized in that, may further comprise the steps:
(1) at SF
6And CO
2Under the mixed gas protected condition, the magnalium starting material are melted fully;
(2) then the Si that wraps with aluminium foil
3N
4Powder is pressed in the magnalium melt;
(3) in melt, add Mg
3N
2Behind the powder, be warming up to 800 ℃-900 ℃ and insulation, to guarantee Si
3N
4Mg in powder and the magnalium melt, Al complete reaction;
(4) insulation is cooled to 680 ℃ after finishing--720 ℃ and insulation, and after stirring melt with graphite disk, drag for the scum silica frost on surface, and water to cast from and obtain the in-situ authigenic aluminium nitride after metal die solidifies and magnesium two silicon strengthen magnesium base composite material.
5. in-situ authigenic aluminium nitride according to claim 4 and magnesium two silicon strengthen method of preparing magnesium-based composite material, it is characterized in that, and in the step (1), described SF
6And CO
2Mixed gas, wherein SF
6Volume accounts for 10%, CO
2Volume accounts for 90%.
6. according to claim 4 or 5 described in-situ authigenic aluminium nitride and magnesium two silicon enhancing method of preparing magnesium-based composite material, it is characterized in that, in the step (1), described fusing, its temperature is controlled between 680 ℃-720 ℃.
7. in-situ authigenic aluminium nitride according to claim 4 and magnesium two silicon strengthen method of preparing magnesium-based composite material, it is characterized in that, and in the step (2), described Si
3N
4Powder, its particle size are 0.5 μ m-45 μ m.
8. in-situ authigenic aluminium nitride according to claim 4 and magnesium two silicon strengthen method of preparing magnesium-based composite material, it is characterized in that, and in the step (3), described insulation, its time is 30 minutes-90 minutes.
9. in-situ authigenic aluminium nitride according to claim 2 and magnesium two silicon strengthen method of preparing magnesium-based composite material, it is characterized in that, and in the step (4), described stirring, its speed is 200r/min-1000r/min.
10. according to claim 4 or 9 described in-situ authigenic aluminium nitride and magnesium two silicon enhancing method of preparing magnesium-based composite material, it is characterized in that, in the step (4), described stirring, its time is 10 minutes-40 minutes.
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|---|---|---|---|
| CNB2007100479444A CN100491566C (en) | 2007-11-08 | 2007-11-08 | In situ self-generation aluminum nitride and magnesium disilicide reinforced magnesium-base composite material and preparation method thereof |
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|---|---|---|---|
| CNB2007100479444A CN100491566C (en) | 2007-11-08 | 2007-11-08 | In situ self-generation aluminum nitride and magnesium disilicide reinforced magnesium-base composite material and preparation method thereof |
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| Publication Number | Publication Date |
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| CN101148722A true CN101148722A (en) | 2008-03-26 |
| CN100491566C CN100491566C (en) | 2009-05-27 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127668A (en) * | 2011-02-22 | 2011-07-20 | 上海交通大学 | Hybrid reinforced magnesium-based composite material of in-situ authigene magnesium oxide and intermetallic compound and preparation method thereof |
| CN103725947A (en) * | 2014-01-09 | 2014-04-16 | 东北大学 | Ceramic particle enhanced magnesium-based composite material and preparation method thereof |
| CN106811643A (en) * | 2017-01-22 | 2017-06-09 | 安徽臣诺机器人科技有限公司 | A kind of handling machinery arm machine pawl and preparation method thereof |
| CN109182856A (en) * | 2018-08-18 | 2019-01-11 | 山东大学 | A kind of AlN and MgB2Particle reinforced magnesium base compound material and preparation method thereof |
| CN115976384A (en) * | 2022-12-30 | 2023-04-18 | 重庆大学 | AlN/AE44 composite material with excellent high-temperature mechanical property and preparation method thereof |
-
2007
- 2007-11-08 CN CNB2007100479444A patent/CN100491566C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127668A (en) * | 2011-02-22 | 2011-07-20 | 上海交通大学 | Hybrid reinforced magnesium-based composite material of in-situ authigene magnesium oxide and intermetallic compound and preparation method thereof |
| CN102127668B (en) * | 2011-02-22 | 2012-10-31 | 上海交通大学 | Hybrid reinforced magnesium-based composite material of in-situ authigene magnesium oxide and intermetallic compound and preparation method thereof |
| CN103725947A (en) * | 2014-01-09 | 2014-04-16 | 东北大学 | Ceramic particle enhanced magnesium-based composite material and preparation method thereof |
| CN103725947B (en) * | 2014-01-09 | 2016-04-13 | 东北大学 | A kind of ceramic particle reinforced magnesium-based composite material and preparation method thereof |
| CN106811643A (en) * | 2017-01-22 | 2017-06-09 | 安徽臣诺机器人科技有限公司 | A kind of handling machinery arm machine pawl and preparation method thereof |
| CN109182856A (en) * | 2018-08-18 | 2019-01-11 | 山东大学 | A kind of AlN and MgB2Particle reinforced magnesium base compound material and preparation method thereof |
| CN109182856B (en) * | 2018-08-18 | 2019-09-17 | 山东大学 | A kind of AlN and MgB2Particle reinforced magnesium base compound material and preparation method thereof |
| CN115976384A (en) * | 2022-12-30 | 2023-04-18 | 重庆大学 | AlN/AE44 composite material with excellent high-temperature mechanical property and preparation method thereof |
| CN115976384B (en) * | 2022-12-30 | 2024-02-23 | 重庆大学 | AlN/AE44 composite material with excellent high-temperature mechanical property and preparation method thereof |
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| CN100491566C (en) | 2009-05-27 |
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Granted publication date: 20090527 Termination date: 20111108 |