CN106834848B - A kind of in-situ particle reinforced magnesium-based composite material and preparation method thereof - Google Patents
A kind of in-situ particle reinforced magnesium-based composite material and preparation method thereof Download PDFInfo
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- CN106834848B CN106834848B CN201710038175.5A CN201710038175A CN106834848B CN 106834848 B CN106834848 B CN 106834848B CN 201710038175 A CN201710038175 A CN 201710038175A CN 106834848 B CN106834848 B CN 106834848B
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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
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
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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
Abstract
The invention discloses a kind of in-situ particle reinforced magnesium-based composite materials and preparation method thereof, belong to metal-base composites preparing technical field.The ammonium salts such as ammonium chloride, ammonium carbonate are added in the magnesium alloy fused mass containing aluminium element by this method, final to obtain nitridation in situ alumina particles enhancing magnesium-based composite material by controlling reaction temperature, stirring intensity and time etc..Generated in-situ aluminum nitride particle size and be evenly distributed, with matrix without interfacial reaction, while its growing amount is controllable.This method is simple for process, flow is short and cost is relatively low, available for high-volume industrial production, has broad application prospects in fields such as aerospace, automobile, 3C.
Description
Technical field：
The present invention relates to a kind of in-situ particle reinforced magnesium-based composite material and preparation method thereof, more particularly to a kind of nitrogen in situ
Change the method for alumina particles enhancing magnesium-based composite material, belong to metal-base composites preparing technical field.
Background technology：
Under the background of increasingly urgent energy-saving and emission-reduction, the fields such as aerospace, automobile, 3C are to lightweight, high tensile metal material
The demand of material is also more and more urgent.Due to particle reinforced magnesium base compound material have high elastic modulus, high specific strength, low-density,
Heat-resist, the advantages that wear resistence is good, it is subject to increasingly extensive research.
Enhancing in particle reinforced magnesium base compound material is mutually generally oxide, carbide or powder metallurgy, such as
Al2O3、SiC、TiC、AlN、Si3N4Deng, these ceramic particles are generally high purity granular, in terms of the preparation process of composite material,
Most of to be added to using techniques such as powder metallurgy or stirring castings in magnesium alloy substrate, there are preparation process complexity, controllabilitys
Difference, hardening constituent particle higher price, the deficiencies of particle and basal body interface associativity are poor, composite material strength is relatively low.And it uses former
The hardening constituent particle that position method is prepared in particle reinforced magnesium base compound material is that forming core in situ is with growing up in metallic matrix, particle tool
Have the advantages that the good clean interfaces wetability between matrix of thermal stability is good and bond strength is high, availability is superior
Performance.
Since aluminium nitride ceramics has high intensity, high rigidity, low-density, low-expansion coefficient, high elastic modulus, high heat conductance
The advantages that, lattice parameter is approached with magnesium, can be good with magnesium alloy substrate compatibility as the substrate of the heterogeneous forming cores of α-Mg.Therefore, nitrogen
Change the preferable enhancing phase that aluminium ceramic particle is magnesium-based composite material.And it is compound to prepare aluminum nitride particle enhancing magnesium-based using in-situ method
Material also becomes one of direction of development.Ye et al., by Mg3N2Powder is added in AM60 magnesium alloy fused mass, passes through the original in melt
Position reaction is prepared for aluminum nitride particle enhancing magnesium-based composite material, but the aluminum nitride particle size generated is larger and is unevenly distributed
Even (Materials Letters, 2004,58:2361-2364).Tyagi et al. leads into the magnesium alloy fused mass containing aluminium element
Enter NH3Gas is also prepared for aluminum nitride particle enhancing magnesium-based composite material (TMS in the melt:Aluminum,2004:63-
72).But above-mentioned preparation method such as prepares aluminium nitride there is also some problem and shortage using addition powder reaction in-situ
Grain enhancing magnesium-based composite material there are reaction speed is slow, reaction not exclusively, aluminum nitride particle size is larger the deficiencies of, and use logical
Enter gas reaction in-situ prepare aluminum nitride particle enhancing magnesium-based composite material there is also nitrogen incorporation ways and reaction unit structure
The deficiencies of complicated.
The above-mentioned deficiency for preparing nitridation in situ alumina particles enhancing magnesium-based composite material method, will influence magnesium-based composite material group
The improvement and the raising of comprehensive performance knitted, and it is unfavorable for large-scale industrial production, so there is certain limitation.
The content of the invention：
The present invention technical purpose be：In view of the deficiencies of the prior art, a kind of in-situ particle reinforced magnesium-based composite wood is provided
The preparation method of material and preparation method thereof, particularly nitridation in situ alumina particles enhancing magnesium-based composite material.
By adding in ammonium salt in containing aluminium-magnesium alloy melt, the reaction in-situ in magnesium alloy fused mass is nitrogenized the present invention
Alumina particles enhance magnesium-based composite material.In composite material preparation process, mechanical agitation and suitable temperature, the control of time are aided in
System can not only shorten the reaction time, improve reaction yield, can also make reaction product evenly.Method of the present invention
Possess magnesium-based composite material can be mass, process simplicity, simple equipments, particle are uniformly dispersed, enhance mutually and matrix circle
The advantages that face is well combined, is environmental-friendly, is at low cost has broad application prospects in fields such as aerospace, automobile, 3C.
The present invention is achieved by the following technical solutions, ammonium salt is added to containing in aluminium-magnesium alloy melt, in setting
Under temperature, time conditions, and it is aided with suitable mechanical agitation, reaction in-situ generates aluminum nitride particle in alloy melt, obtains
The magnesium-based composite material of nitridation in situ alumina particles enhancing and final cast molding.Composite material is by matrix and enhancing phase composition, base
Body is the magnesium alloy containing aluminium element, and enhancing is mutually aluminum nitride particle.
A kind of preparation method of in-situ particle reinforced magnesium-based composite material of the present invention, step include as follows：
(1) magnesium alloy ingot containing Al is inserted in crucible, heating and melting is to liquid under the conditions of gas shield；
(2) magnesium alloy fused mass is controlled to add in melt a certain amount of ammonium salt to design temperature, and use agitating device pair
Melt is stirred；
(3) melt surface layer scum silica frost is removed, melt is poured and is cast from metal pattern or sand mo(u)ld, obtains the enhancing of nitridation in situ alumina particles
Magnesium-based composite material.
Preferred processing condition is as follows：
The content of aluminium element is 6-25wt.% in magnesium alloy ingot described in step (1).
Design temperature described in step (2) is higher than 10~100 DEG C of magnesium alloy fused mass liquidus temperature.
Ammonium salt described in step (2) is anhydrous ammonium chloride or Carbon Dioxide ammonium, and the purity of ammonium salt is not less than
95.0wt.%.
Ammonium salt addition described in step (2) is 5~30wt.% of melt quality.
Agitating device rotating speed described in step (2) is 100~1000rpm, and mixing time is 5~60min.
The magnesium alloy of above-mentioned steps (1) is the arbitrarily magnesium alloy containing Al, as element includes the conjunction of Al, Zn, Mn, Si, Mg
Gold；Alloy including Al, Mn, Si, Mg element etc..
Preparation method used in the present invention has the following advantages that：In containing aluminium-magnesium alloy melt, the ammonium of Nitrogen element is utilized
Salt prepares aluminum nitride particle enhancing magnesium-based composite material using reaction in-situ.Generated in-situ aluminum nitride particle size it is small and
It is evenly distributed, is high without interfacial reaction, interface bond strength with matrix, and its growing amount is controllable, can obtain original of good performance
Position aluminum nitride particle enhancing magnesium-based composite material.This method is simple, flow is short and cost is relatively low, can high-volume industrial production, tool
Have broad application prospects.
Description of the drawings：
Fig. 1 is the preparation technology flow chart of in-situ particle reinforced magnesium-based composite material.
Fig. 2 is the SEM image of in-situ particle reinforced magnesium-based composite material in embodiment 2.
Fig. 3 is the SEM image of in-situ particle reinforced magnesium-based composite material in embodiment 5.
Specific embodiment：
It is further illustrated the present invention below in conjunction with specific case study on implementation, it is pointed out that：Following case study on implementation is only used
In the specific implementation method for illustrating the present invention, rights protection scope of the present invention can not be limited.
Embodiment 1：
The preparation method of present embodiment in-situ particle reinforced magnesium-based composite material carries out according to the following steps：
(1) by 500g magnesium alloys (ingredient 6.0wt.%Al, 0.74wt.%Zn, 0.01wt.%Mn, 0.01wt.%Si,
Surplus is Mg) alloy inserted in crucible, in N2+SF6Heating and melting is to liquid under gaseous mixture protective condition.
(2) magnesium alloy fused mass is controlled to 625 DEG C (this temperature is higher than 10 DEG C of melt liquidus curve), 25g Carbon Dioxide ammoniums is (pure
Spend for 95.0wt.%) it adds in melt, while using stirring slurry with the melt 5min of the rotating speed stirring molten condition of 100rpm.
(3) melt heating temperature fishes for bath surface slag, pours and cast from sand mo(u)ld to about 680 DEG C, obtains nitridation in situ aluminium
Particle reinforced magnesium base compound material.
Embodiment 2：
The preparation method of present embodiment in-situ particle reinforced magnesium-based composite material carries out according to the following steps：
(1) by magnesium alloy (ingredient 9.7wt.%Al, 1.1wt.%Zn, 0.02wt.%Mn, 0.01wt.% of 500g
Si, surplus Mg) alloy inserted in crucible, in CO2+SF6Heating and melting is to liquid under gaseous mixture protective condition.
(2) magnesium alloy fused mass is controlled to 693 DEG C (this temperature is higher than 100 DEG C of melt liquidus curve), by 50g anhydrous ammonium chlorides
(purity 99.0wt.%) is added in melt, while using stirring slurry with the melt of the rotating speed stirring molten condition of 500rpm
15min。
(3) melt heating temperature fishes for bath surface slag, pours and cast from metal pattern to about 670 DEG C, obtains nitridation in situ
Alumina particles enhance magnesium-based composite material.
Embodiment 3：
The preparation method of present embodiment in-situ particle reinforced magnesium-based composite material carries out according to the following steps：
(1) by magnesium alloy (ingredient 18.5wt.%Al, 0.5wt.%Zn, 0.02wt.%Mn, 0.02wt.% of 500g
Si, surplus Mg) alloy inserted in crucible, in N2+SF6Heating and melting is to liquid under gaseous mixture protective condition.
(2) magnesium alloy fused mass is controlled to 585 DEG C (this temperature is higher than 30 DEG C of melt liquidus curve), by 100g Carbon Dioxide ammoniums
(purity 99.5wt.%) is added in melt, while using stirring slurry with the melt of the rotating speed stirring molten condition of 800rpm
40min。
(3) melt heating temperature fishes for bath surface slag, pours and cast from sand mo(u)ld to about 600 DEG C, obtains nitridation in situ aluminium
Particle reinforced magnesium base compound material.
Embodiment 4：
The preparation method of present embodiment in-situ particle reinforced magnesium-based composite material carries out according to the following steps：
(1) by the magnesium alloy (ingredient 25.0wt.%Al, 0.03wt.%Mn, 0.02wt.%Si, surplus Mg) of 500g
Alloy is inserted in crucible, in CO2+SF6Heating and melting is to liquid under gaseous mixture protective condition.
(2) magnesium alloy fused mass is controlled to 570 DEG C (this temperature is higher than 60 DEG C of melt liquidus curve), by 150g anhydrous ammonium chlorides
(purity 95.0wt.%) is added in melt, while using stirring slurry with the melt of the rotating speed stirring molten condition of 1000rpm
60min。
(3) melt heating temperature fishes for bath surface slag, pours and cast from metal pattern to about 585 DEG C, obtains nitridation in situ
Alumina particles enhance magnesium-based composite material.
Embodiment 5：
The preparation method of present embodiment in-situ particle reinforced magnesium-based composite material carries out according to the following steps：
(1) by the magnesium alloy (ingredient 12.8wt.%Al, 0.01wt.%Mn, 0.02wt.%Si, surplus Mg) of 500g
Alloy is inserted in crucible, in CO2+SF6Heating and melting is to liquid under gaseous mixture protective condition.
(2) magnesium alloy fused mass is controlled to 625 DEG C (this temperature is higher than 40 DEG C of melt liquidus curve), 75g Carbon Dioxide ammoniums is (pure
Spend for 98.0wt.%) it adds in melt, while using stirring slurry with the melt 30min of the rotating speed stirring molten condition of 900rpm.
(3) melt heating temperature fishes for bath surface slag, pours and cast from sand mo(u)ld to about 650 DEG C, obtains nitridation in situ aluminium
Particle reinforced magnesium base compound material.
Although listing in detail here and illustrating that case is preferably implemented, skilled person will appreciate that, can it is not taking off
Carried out in the case of from marrow of the present invention it is various improve, addition, the modes such as replace, these contents are all identified as belonging to right will
It asks within limited the scope of the present invention.
Claims (5)
1. a kind of preparation method of in-situ particle reinforced magnesium-based composite material, which is characterized in that comprise the following steps：
(1) magnesium alloy ingot containing Al is inserted in crucible, heating and melting is to liquid under the conditions of gas shield；
(2) magnesium alloy fused mass is controlled to add in melt a certain amount of ammonium salt to design temperature, and use agitating device to melt
It is stirred；
(3) melt surface layer scum silica frost is removed, melt is poured and is cast from metal pattern or sand mo(u)ld, obtains nitridation in situ alumina particles enhancing magnesium-based
Composite material；
Design temperature described in step (2) is higher than 10~100 DEG C of magnesium alloy fused mass liquidus temperature；Described in step (2)
Ammonium salt be anhydrous ammonium chloride or Carbon Dioxide ammonium；Ammonium salt addition described in step (2) for melt quality 5~
30wt.%.
2. the preparation method of in-situ particle reinforced magnesium-based composite material according to claim 1, which is characterized in that step
(1) content of aluminium element is 6-25wt.% in the magnesium alloy ingot described in.
3. the preparation method of in-situ particle reinforced magnesium-based composite material according to claim 1, which is characterized in that step
(2) purity of ammonium salt is not less than 95.0wt.% in.
4. the preparation method of in-situ particle reinforced magnesium-based composite material according to claim 1, which is characterized in that step
(2) the agitating device rotating speed described in is 100~1000rpm, and mixing time is 5~60min.
5. the in-situ particle reinforced magnesium-based composite material that any one the method according to Claims 1 to 4 is prepared.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148723A (en) * | 2007-11-08 | 2008-03-26 | 上海交通大学 | In situ self-generation aluminum nitride enhanced magnesium-base composite material and preparation method thereof |
| 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 |
| CN106048351A (en) * | 2016-08-04 | 2016-10-26 | 北京工业大学 | Preparation method of AIN particle-reinforced magnesium-based composite material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2866917B2 (en) * | 1994-10-05 | 1999-03-08 | 工業技術院長 | Superplasticity Development Method for Ceramic Particle Reinforced Magnesium Matrix Composite by Melt Stirring Method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148723A (en) * | 2007-11-08 | 2008-03-26 | 上海交通大学 | In situ self-generation aluminum nitride enhanced magnesium-base composite material and preparation method thereof |
| 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 |
| CN106048351A (en) * | 2016-08-04 | 2016-10-26 | 北京工业大学 | Preparation method of AIN particle-reinforced magnesium-based composite material |
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