CN103834840A - Novel flame-retardant and heat-resistant high-strength magnesium-based material and preparation method thereof - Google Patents
Novel flame-retardant and heat-resistant high-strength magnesium-based material and preparation method thereof Download PDFInfo
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- CN103834840A CN103834840A CN201410091897.3A CN201410091897A CN103834840A CN 103834840 A CN103834840 A CN 103834840A CN 201410091897 A CN201410091897 A CN 201410091897A CN 103834840 A CN103834840 A CN 103834840A
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Abstract
The invention discloses a novel flame-retardant and heat-resistant high-strength magnesium-based material and a preparation method thereof, and belongs to the field of preparation of a metal material. Ca is 0.5-5% of mass of a magnesium-aluminum alloy; the volume fraction of an SiC particle accounts for 1-15% of that of the magnesium-aluminum alloy; the chemical ingredients of the magnesium-aluminum alloy comprise 1-9% of aluminum, 1% of zinc and the balance of Mg; the particle size of the SiC particles is smaller than or equal to 10mu m. By adopting the novel flame-retardant and heat-resistant high-strength magnesium-based material, the inoxidizability, the high-temperature behavior and the creep property of the magnesium-based composite material can be effectively improved, the corrosion resistance of the magnesium-based composite material also can be improved, and the novel flame-retardant and heat-resistant high-strength magnesium-based material has a certain refining effect on crystalline grains.
Description
Technical field
The preparation method who the present invention relates to a kind of novel flame-retardant heat-resistance high-strength mg-based material, belongs to metal material field.
Background technology
In order to reduce the consumption of automobile fuel and the discharge of pollutent, magnesium and alloy thereof as the lightest metallic substance of occurring in nature the application in automotive industry more and more, particularly Mg-Al is associated gold.Magnesium base composite material is oxidizable, solidity to corrosion is poor, high-temperature behavior and creep property poor.In the time that use temperature exceedes 150 ℃, Mg-Al is associated golden intensity and sharply declines, and has limited its use range, for meeting the component such as automobile demand to light material under middle high-temperature work environment, the exploitation of high temperature resistant high strength and low cost mg-based material, significant.
Summary of the invention
The object of the invention is the situation for background technology, adopt a kind of method of casting+stirring+hot pressing, make a kind of new magnesium base composite material, make it have higher oxidation-resistance, high-temperature behavior, creep property and erosion resistance, expand the range of application of mg-based material.
Technical scheme of the present invention is: a kind of novel flame-retardant heat-resistance high-strength mg-based material, and the quality of Ca accounts for the 0.5%-5% of magnalium quality; The volume fraction of SiC particle accounts for the 1%-15% of magnalium volume; Therefore the quality of calcium and SiC is to be determined by magnalium.The chemical composition of described magnalium is that Al is (1%-9%), and all the other are Mg; Particle diameter≤10 μ the m of SiC particle;
A kind of preparation method of novel flame-retardant heat-resistance high-strength mg-based material comprises the steps:
(1) in the HF acid distillation aqueous solution that is 7.6% by SiC particle in concentration, soak 24 hours, then with distilled water, the washing of SiC particle is extremely neutral, in drying baker, dry subsequently, filter out needed SiC particle size;
(2) SiC particle is put into stoving oven, furnace temperature is transferred to 600 ℃, drying time is 120min;
(3) in smelting pot, be sprinkled into insulating covering agent (being 3 ‰ of magnalium weight-5 ‰), then put into magnalium piece, and on magnalium piece, spread one deck insulating covering agent (being 2 ‰ of magnalium weight-4 ‰), temperature is adjusted to 720 ℃ afterwards; Pure Ca is carried out to preheating with being placed on smelting furnace top on Aluminium Foil Package simultaneously; Above-mentioned insulating covering agent is by MgCl
2, KCl, NaCl, CaCl
2, BaCl
2composition, mass percent is respectively 38%, 37%, 8%, 8%, 9%, spreading insulating covering agent is mainly the oxidation in order to prevent material;
(4), in the time that magnalium piece has just started to melt, (protection gas composition is SF just to pass into immediately shielding gas
6+ CO
2gas volume is than being 1:100), be fused into completely after liquid until magnalium piece;
(5) the pure Ca of preheating is put into crucible, treat that it all melts;
(6) smelting furnace temperature is adjusted to 592 ℃ ± 5 ℃, be down to after 592 ℃ ± 5 ℃ until the temperature of magnalium solution in crucible, skim, remove surperficial oxide inclusion, then stirring rake is dropped to the mid-way of liquation, start stirrer and stir, form after eddy current at bath surface, add fast and be preheating to the SiC particle that 600 ℃ of volume fractions are 1%-15%, then stir 25min under semi-solid state, then be warmed up to 750 ℃ and be incubated 5min.Stop stirring, take out crucible, be poured in the middle of the mould that is preheating to 400 ℃;
(7) take out ingot casting, make ingot casting in air, naturally cool to room temperature;
(8) by the SiC particle reinforced magnesium base compound material line cutting sample preparation making, pressing material length is 50mm, and clean with sand papering;
(9) pressing material being put into furnace temperature is to be incubated after 30min in the holding furnace of 420 ℃, put into extrusion mould and carry out extrusion molding, and the hydropress that extrusion equipment is 200t, extruding rate is 3mm/s.
effect of the present invention is:
The magnesium base composite material that the present invention adds Ca and SiC particle to make in magnalium, can significantly improve its high-temperature behavior, flame retardant resistance and solidity to corrosion, add the distribution of the material second-phase compared with not adding the material of SiC particle after SiC particle that change has occurred, second-phase does not mainly distribute along crystal boundary, but be mainly distributed on the surface and matrix of SiC particle, what after hot extrusion, second-phase distributed is more even.Because as cast condition magnesium base composite material exists coarse grains, shrinkage cavity and the defect such as loose, can produce adverse influence to its performance, therefore need it to carry out hot extrusion, not only can crystal grain thinning, and can make Second Phase Particle more tiny evenly, strengthening effect is more obvious, further improves its mechanical property, significant for the range of application that expands mg-based material.
The magnesium base composite material containing calcium constituent that the present invention makes by casting+stirring+hot extrusion can effectively improve oxidation-resistance, high-temperature behavior and the creep property of magnesium base composite material, but also can improve the solidity to corrosion of magnesium base composite material, and crystal grain is had to certain refining effect, is a kind of preparation method of very good novel flame-retardant heat-resistance high-strength mg-based material; Be conducive to expand the use in middle high temperature of the use range of mg-based material, particularly mg-based material.
Embodiment
embodiment:the weight of magnalium is 1000g; The content of Ca is that the median size of 3%, SiC particle is that 5 μ m, volume fraction are 10%.
Preparation method:
One, material is prepared
1. the quality of determining magnalium is 1000g, and the content that the content that this time experiment magnalium used is AZ91(Al is 9%, Zn is 1%, and all the other are Mg);
The preparation of 2.SiC particle
1) in the HF acid distillation aqueous solution that is 7.6% to micron SiC particle in concentration, soak 24 hours, then with distilled water, the washing of SiC particle is extremely neutral, in drying baker, dry subsequently, filtering out needed median size is the SiC particle of 5 μ m;
2) calculate the quality of required SiC according to the size of the quality of magnalium and the SiC particle selected, the fundamental formular of calculating is:
This prepares magnalium used is AZ91 alloy (content that the content of Al is 9%, Zn is 1%, and all the other are Mg), and its density is 1.81g/cm
3, the density of SiC particle is 3.19 g/cm
3, the quality that calculates SiC particle is:
Mp=196g
The preparation of 3.Ca
1) Ca adds with the form of pure calcium, is that 3% quality that calculates required Ca is 30g according to the massfraction of the quality of magnalium and determined Ca;
Two, the preparation of as cast condition material
1. casting equipment is assembled, and debug before casting material;
2. resistance furnace is warmed up to 700 ℃, after insulation for some time, cleaning crucible; Mould is placed in to process furnace simultaneously and carries out preheating, 400 ℃ ± 5 ℃ of preheating temperatures; SiC particle is put into stoving oven, furnace temperature is transferred to 600 ℃, drying time is 120min;
3. in smelting pot, be sprinkled into 3-5g insulating covering agent, then put into magnalium piece, and on magnalium piece, spread one deck insulating covering agent (2-4g), temperature is adjusted to 720 ℃ afterwards; Pure Ca is carried out to preheating with being placed on smelting furnace top on Aluminium Foil Package simultaneously; Above-mentioned insulating covering agent is by MgCl
2, KCl, NaCl, CaCl
2, BaCl
2composition mass percent is respectively 38%, 37%, 8%, 8%, 9%, and spreading insulating covering agent is mainly the oxidation in order to prevent material;
4. in the time that magnalium starts to melt, (protection gas composition is SF just to pass into immediately shielding gas
6+ CO
2gas gas volume is than being 1:100), treat that magnalium piece is fused into liquid completely;
5. the pure Ca of preheating is put into crucible, treat that it all melts;
6. smelting furnace temperature is adjusted to 592 ℃ ± 5 ℃, be down to after 592 ℃ ± 5 ℃ until magnalium solution in crucible, skim, remove surperficial oxide inclusion, then stirring rake is dropped to the mid-way of melt, start stirrer and stir, form suitable eddy current at bath surface, add fast and be preheating to the SiC particle that 600 ℃ of quality are 196g, then stir 25min under semi-solid state, then be incubated 5min after being warmed up to 750 ℃.Stop stirring, take out crucible, be poured in the middle of the mould that is preheating to 400 ℃;
7. take out ingot casting, make ingot casting in air, naturally cool to room temperature; The magnesium base composite material casting out in this example is that diameter is the bar of 40mm;
8. collator
Three, the hot extrusion of as cast condition material
1. by the SiC particle reinforced magnesium base compound material line cutting sample preparation making, pressing material length is 50mm, and clean with sand papering;
2. extrusion equipment and extrusion mould are assembled, and debugging in advance, squeezing device comprises pressure head, extruding cushion block, compression sleeve, bar to be processed, Extruding die; Extruding die is arranged in compression sleeve, and bar to be processed is arranged on above Extruding die, is provided with extruding cushion block above bar to be processed, and pressure head is arranged on above extruding cushion block.By make bar to be processed be under pressure and extrusion molding to ram pressures.
3. mould is put into preheating oven, furnace temperature is set as to 420 ℃, it is that the holding furnace of 420 ℃ is incubated 30min that the bar of extruding need be put into preheating temperature;
4 after soaking time arrives, and pressing material is taken out and put into from preheating oven extrusion mould, opens extrusion equipment and pushes;
5. after having pushed, disconnecting power switch, rises pressing machine, takes out the section bar squeezing out from extrusion mould, and this prepares the hydropress that extrusion equipment used is 200t, and extruding rate is 3mm/s.
In embodiment, the bar that cuts down is hot extruded into the bar that diameter is 10mm, extrusion ratio is 16:1.
Claims (2)
1. a novel flame-retardant heat-resistance high-strength mg-based material, the quality of Ca accounts for the 0.5%-5% of magnalium quality; The volume fraction of SiC particle accounts for the 1%-15% of magnalium volume; The chemical composition of described magnalium is that aluminium is 1%-9%, zinc be 1% all the other are Mg; Particle diameter≤10 μ the m of SiC particle.
2. a preparation method for novel flame-retardant heat-resistance high-strength mg-based material, comprises the steps:
(1) in the HF acid distillation aqueous solution that is 7.6% by SiC particle in concentration, soak 24 hours, then with distilled water, the washing of SiC particle is extremely neutral, in drying baker, dry subsequently, filter out needed SiC grain diameter≤10 μ m;
(2) SiC particle is put into stoving oven, furnace temperature is transferred to 600 ℃, drying time is 120min;
(3) in smelting pot, be sprinkled into insulating covering agent, insulating covering agent is 3 ‰ of magnalium weight-5 ‰, then puts into magnalium piece, and spreads one deck insulating covering agent on magnalium piece, and insulating covering agent is 2 ‰ of magnalium weight-4 ‰, temperature is adjusted to 720 ℃ afterwards; Pure Ca is carried out to preheating with being placed on smelting furnace top on Aluminium Foil Package simultaneously; Described insulating covering agent is that mass percent is MgCl
2be 38%; KCl is 37%; NaCl is 8%; CaCl
2be 8%; BaCl
2be 9%;
(4) in the time that magnalium starts to melt, pass into immediately shielding gas, shielding gas composition is SF
6+ CO
2; Gas volume is than being SF
6: CO
2=1:100, treats that magnalium piece is fused into liquid completely;
(5) the pure Ca of preheating is put into crucible, treat that it all melts;
(6) smelting furnace temperature is adjusted to 592 ℃ ± 5 ℃, be down to after 592 ℃ ± 5 ℃ until the temperature of magnalium solution in crucible, skim, remove surperficial oxide inclusion, start stirrer and stir, make bath surface form eddy current, add the SiC particle that 600 ℃ of volume fractions are 1%-15%, stir 25min, be then warmed up to 750 ℃ and be incubated 5min; Stop stirring, take out crucible, be poured in the middle of the mould that is preheating to 400 ℃;
(7) take out ingot casting, make ingot casting in air, naturally cool to room temperature;
(8) the SiC particle reinforced magnesium base compound material line cutting sample preparation making being become to length is 50mm pressing material, and clean with sand papering;
(9) pressing material being put into furnace temperature is to be incubated 30min in the holding furnace of 420 ℃, put into extrusion mould and carry out extrusion molding, and the hydropress that extrusion equipment is 200t, extruding rate is 3mm/s.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106366688A (en) * | 2016-08-26 | 2017-02-01 | 山东天汇防水材料有限公司 | Flame retardant coiled material and preparation method thereof |
| CN107803408A (en) * | 2017-10-26 | 2018-03-16 | 河南工业大学 | A kind of preparation method for strengthening composite using second-phase strength SiC particulate |
| CN110317984A (en) * | 2019-07-04 | 2019-10-11 | 重庆电子工程职业学院 | A kind of antiflaming magnesium alloy composite material and preparation method with excellent toughness |
| CN115433862A (en) * | 2022-08-05 | 2022-12-06 | 太原理工大学 | Preparation method of Ni-free degradable magnesium-based material |
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| CN101748306A (en) * | 2008-12-02 | 2010-06-23 | 苏州有色金属研究院有限公司 | Multiphase ceramic hybrid composite reinforced metal matrix composite material and preparation process thereof |
| CN101880788A (en) * | 2010-06-02 | 2010-11-10 | 太原理工大学 | Method for enhancing SiC particle grinding of magnesium aluminum alloy |
| CN103014387A (en) * | 2012-12-24 | 2013-04-03 | 中北大学 | Preparation method of magnesium base composite doped with SiC grains |
| JP2013514463A (en) * | 2011-01-11 | 2013-04-25 | コリア・インスティテュート・オブ・マシナリー・アンド・マテリアルズ | Magnesium alloy having excellent ignition resistance and mechanical properties and method for producing the same |
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2014
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Patent Citations (4)
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| CN101748306A (en) * | 2008-12-02 | 2010-06-23 | 苏州有色金属研究院有限公司 | Multiphase ceramic hybrid composite reinforced metal matrix composite material and preparation process thereof |
| CN101880788A (en) * | 2010-06-02 | 2010-11-10 | 太原理工大学 | Method for enhancing SiC particle grinding of magnesium aluminum alloy |
| JP2013514463A (en) * | 2011-01-11 | 2013-04-25 | コリア・インスティテュート・オブ・マシナリー・アンド・マテリアルズ | Magnesium alloy having excellent ignition resistance and mechanical properties and method for producing the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106366688A (en) * | 2016-08-26 | 2017-02-01 | 山东天汇防水材料有限公司 | Flame retardant coiled material and preparation method thereof |
| CN107803408A (en) * | 2017-10-26 | 2018-03-16 | 河南工业大学 | A kind of preparation method for strengthening composite using second-phase strength SiC particulate |
| CN110317984A (en) * | 2019-07-04 | 2019-10-11 | 重庆电子工程职业学院 | A kind of antiflaming magnesium alloy composite material and preparation method with excellent toughness |
| CN115433862A (en) * | 2022-08-05 | 2022-12-06 | 太原理工大学 | Preparation method of Ni-free degradable magnesium-based material |
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| CN103834840B (en) | 2016-01-27 |
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Effective date of registration: 20220420 Address after: 043899 No. 20, Dayun Road, Beicheng District, Wenxi County, Yuncheng City, Shanxi Province Patentee after: SHANXI YINGUANG HUASHENG MAGNESIUM INDUSTRY CO.,LTD. Address before: 030024 No. 79 West Main Street, Wan Berlin District, Shanxi, Taiyuan, Yingze Patentee before: Taiyuan University of Technology |