EP3553199B1 - Procédé de préparation de matériau composite à base de magnésium renforcé mélange par du magnésium-zinc-yttrium quasi-cristal et du carbure de bore - Google Patents
Procédé de préparation de matériau composite à base de magnésium renforcé mélange par du magnésium-zinc-yttrium quasi-cristal et du carbure de bore Download PDFInfo
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- EP3553199B1 EP3553199B1 EP19153314.0A EP19153314A EP3553199B1 EP 3553199 B1 EP3553199 B1 EP 3553199B1 EP 19153314 A EP19153314 A EP 19153314A EP 3553199 B1 EP3553199 B1 EP 3553199B1
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- magnesium
- furnace
- vacuum
- frequency induction
- medium frequency
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- 239000011777 magnesium Substances 0.000 title claims description 67
- 229910052580 B4C Inorganic materials 0.000 title claims description 33
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims description 30
- 239000002131 composite material Substances 0.000 title claims description 27
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims description 18
- 229910052749 magnesium Inorganic materials 0.000 title claims description 18
- PEEFQZLSNAERDY-UHFFFAOYSA-N [Mg].[Zn].[Y] Chemical compound [Mg].[Zn].[Y] PEEFQZLSNAERDY-UHFFFAOYSA-N 0.000 title claims description 16
- 239000013079 quasicrystal Substances 0.000 title claims description 15
- 238000000034 method Methods 0.000 title claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 66
- 230000006698 induction Effects 0.000 claims description 41
- 238000002844 melting Methods 0.000 claims description 41
- 230000008018 melting Effects 0.000 claims description 41
- 229910052786 argon Inorganic materials 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000011701 zinc Substances 0.000 claims description 24
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- 238000009716 squeeze casting Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 239000010439 graphite Substances 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 229910052725 zinc Inorganic materials 0.000 claims description 12
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 11
- 238000003723 Smelting Methods 0.000 claims description 11
- 238000007664 blowing Methods 0.000 claims description 11
- MIOQWPPQVGUZFD-UHFFFAOYSA-N magnesium yttrium Chemical compound [Mg].[Y] MIOQWPPQVGUZFD-UHFFFAOYSA-N 0.000 claims description 11
- 238000007669 thermal treatment Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 235000019353 potassium silicate Nutrition 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 238000005266 casting Methods 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 239000011888 foil Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000010907 mechanical stirring Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000002441 X-ray diffraction Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910001868 water Inorganic materials 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229910003243 Na2SiO3·9H2O Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 238000005275 alloying Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 230000002431 foraging effect Effects 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000012982 microporous membrane Substances 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims description 2
- 230000008023 solidification Effects 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 230000003746 surface roughness Effects 0.000 claims description 2
- 238000009864 tensile test Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- 238000010586 diagram Methods 0.000 description 5
- 238000012876 topography Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000946 Y alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
Images
Classifications
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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
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D18/00—Pressure casting; Vacuum casting
- B22D18/02—Pressure casting making use of mechanical pressure devices, e.g. cast-forging
-
- 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
-
- 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
-
- 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
- C22C1/1073—Infiltration or casting under mechanical pressure, e.g. squeeze casting
-
- 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
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
-
- 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
- C22C32/0052—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 carbides
- C22C32/0057—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 carbides based on B4C
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
Definitions
- the present invention relates to a method of preparing magnesium-zinc-yttrium quasicrystal and boron carbide mixed enforced Mg-based composite materials, which belong to the technical area of preparing and applying the non-ferrous metal materials.
- the magnesium alloy materials have widely applied in the automobile and aerospace area for it they are characterized in low density, high specific strength, excellent shock resistance, strong electromagnetic shielding capability and easy processing. However, the application of magnesium alloy in the industrial area is restricted for its low hardness, low anti-tensile strength and poor corrosion resistance.
- the Chinese patent CN 102618766B discloses a method of producing a quasicrystal enhanced Mg-Zn-Y alloy by means of conventional melting and subsequent thermal treatment.
- the quascicrystal has high hardness, high elastic modules, low expansion coefficient and excellent corrosion resistance, it is extremely suitable to be used as the enhance phase of the magnesium alloy and can efficiently improve the mechanical property of the magnesium alloy.
- the boron carbide particles are of great application potential for they have low density, excellent chemical stability, abrasive resistance and can be evenly distributed in the magnesium substrate with a stable interface.
- mixed particles reinforced Mg-based composite materials are still in the research phase and the process technology needs to be improved.
- the present invention is done based on the situations introduced by the background art and aims at improving the mechanical property of the magnesium alloy by adopting the magnesium alloy as the substrate, the endogenous magnesium-zinc-yttrium quasicrystal and boron carbide as the reinforced phase, via smelting in the vacuum medium frequency induction melting furnace and then squeezing casting to prepare magnesium-zinc-yttrium quasicrystal and boron carbide mixed reinforced Mg-based composite materials.
- Chemical materials used in the present invention are: magnesium, zinc, magnesium yttrium interalloy, boron carbide, zinc oxide, talcum powder, water glass, deionized water, aluminum foil, absolute alcohol, argon, their amounts used in the composition are: (measured in gram, milliliter and centimeter 3 ): magnesium Mg 4127g ⁇ 0.1g Zinc Zn 784g ⁇ 0.1g magnesium yttrium interalloy Mg 89 Y 11 571g ⁇ 0.1g boron carbide B 4 C 300g ⁇ 0.1g zinc oxide ZnO 80g ⁇ 1g talcum powder Mg 3 Si 4 O 10 ](OH) 2 50g ⁇ 1g water glass Na 2 SiO 3 ⁇ 9H 2 O 25g ⁇ 1g deionized water H 2 O 1000mL ⁇ 50mL aluminum foil Al 300mm ⁇ 0.5mm ⁇ 300mm absolute alcohol C 2 H 5 OH 3500mL ⁇ 50mL argon Ar 800000cm 3 ⁇ 100 cm 3 the preparation method comprises:
- magnesium-zinc-yttrium quasicrystal and boron carbide mixed reinforced Mg-based composite materials are prepared by adopting the magnesium alloy as the substrate, the endogenous magnesium-zinc-yttrium quasicrystal and boron carbide as the reinforced phase, via smelting in the vacuum medium frequency induction melting furnace, protection of bottom blowing argon, mechanical stirring, squeeze casting and heat-treatment.
- the preparation method has advanced process and strict procedures, wherein the data is accurate and detailed, and the prepared Mg-based composite materials have 315MPa tensile strength, 7% elongation, 108Hv hardness, making it an advanced preparation method of mixed reinforced Mg-based composite materials.
- Figure 1 shows the smelting state diagram of the Mg-based composite materials, wherein the location and connection relationship of each part should be correct and the ratio is conducted according to the amount and the process should be conducted according to the sequence.
- the amount of the chemical materials used in the preparation of smelting is determined by the pre-configured scope, and they are measured in gram, milliliter and centimeter 3 .
- the smelting of Mg-based composite materials is conducted in the vacuum medium frequency induction melting furnace, and finished by the process of mediate frequency induction heating, bottom blowing argon and mechanical stirring.
- the vacuum medium frequency induction melting furnace is a vertical one.
- the bottom of the vacuum medium frequency induction melting furnace 1 is a furnace base 2, and the inside of the vacuum medium frequency induction melting furnace 1 is a furnace chamber 3; a worktable 6 is configured in the bottom of the furnace chamber 3 and a graphite melting crucible 7 is put on the worktable 6.
- the outside of the graphite melting crucible 7 is surrounded by the medium frequency induction heater 8 and the inside of the graphite melting crucible 7 is the alloy melt 9; an outlet pipe 4 is configured on the top right of the vacuum medium frequency induction melting furnace 1 and it is controlled by the outlet valve 5; the argon bottle 15 is configured on the top left of the vacuum medium frequency induction melting furnace 1 and an argon pipe 16 and an argon valve 17 are configured on the argon bottle 15.
- the argon pipe 16 is connected to the bottom blow motor 11.
- the bottom blow motor 11 is connected to the bottom blow pipe 12.
- the bottom blow pipe 12 communicates to the graphite melting crucible 7 through the furnace base 2 and worktable 6 and bottom blows the alloy melt 9;
- a vacuum pump 13 is configured in the bottom right of the furnace base 2 and communicates to the furnace chamber 3 through a vacuum pipe 14;
- a feed pipe 27, a feed valve 28 and a mechanical agitator 29 are configured on the top of the vacuum medium frequency induction melting furnace 1 and the feed pipe 27 and the mechanical agitator 29 extends to the graphite melt crucible 7 through the furnace top base.
- a electric cabinet 18 is configured on the right of the vacuum medium frequency induction melting furnace 1 and a display screen 19, an indicator light 20, a power switch 21, a medium frequency induction heating controller 22, a bottom blow motor controller 23 and a vacuum pump controller 24 are configured on the electric cabinet 18; the electric cabinet 18 is connected to the medium frequency induction heater 8 through a first cable 25; The electric cabinet 18 is connected to the bottom blow motor 11 and a vacuum pump 13 through the second cable 26; the furnace cavity 3 is filled with argon 10.
- FIG. 2 it shows the metallographic structure diagram of Mg-based composite materials, wherein there are no defects such as inclusion and air holes in the metallographic structure diagram and the quascicrystal phase Mg 3 Zn 6 Y and boron carbide particles can be evenly distributed in particles.
- FIG. 3 shows the fracture topography of Mg-based composite materials, wherein massive small dimples exist in the fracture topography and it demonstrates that it has excellent plasticity.
- FIG. 4 it shows X-ray diffraction intensity spectrum of Mg-based composite materials.
- the ordinate is diffraction intensity index and the abscissa is the diffraction angle 2 ⁇ . It can be seen that mainly ⁇ -Mg substrate magnesium phase, Mg 3 Zn 6 Y quascicrystal phase and B 4 C reinforced phase exist in Mg-based composite materials.
Claims (2)
- Procédé de préparation de matériaux composites à base de Mg renforcés par mélange de quasi-cristaux magnésium-zinc-yttrium et de carbure de bore, caractérisé en ce que les matériaux chimiques utilisés sont : magnésium, zinc, alliage magnésium-yttrium, carbure de bore, oxyde de zinc, poudre de talc, verre soluble étant une eau déminéralisée Na2SiO3·9H2O, papier d'aluminium, alcool pur, argon, avec les teneurs suivantes :
magnésium Mg 4127 g ± 0,1 g zinc Zn 784 g ± 0,1 g alliage magnésium-yttrium Mg89Y11 571 g ± 0,1 g carbure de bore B4C 300 g ± 0,1 g oxyde de zinc ZnO 80 g ± 1 g poudre de talc Mg3[Si4O10](OH)2 50 g ± 1 g verre soluble Na2SiO3·9H2O 25 g ± 1 g eau déminéralisée H2O 1000 ml ± 50 ml papier d'aluminium Al 300 mm × 0,5 mm × 300 mm alcool pur C2H5OH 3500 ml ± 50 ml argon Ar 800000 cm3 ± 100 cm3 (1) la préparation du moule de coulée
le moule de coulée sous pression de type fermé-ouvert est fabriqué par usinage à chaud d'acier à matrices avec une cavité rectangulaire, la cavité ayant une grandeur de 200 mm × 160 mm × 90 mm et la rugosité de surface Ra de la cavité étant comprise entre 0,08 et 0,16 µm ;(2) la préparation de l'agent de revêtement
pesée d'oxyde de zinc 80 g ± 1 g, de poudre de talc 50 g ± 1 g, de verre soluble 25 g ± 1 g, mesure d'eau déminéralisée 300 ml ± 1 ml, ajout d'oxyde de zinc 80 g ± 1 g, de poudre de talc 50 g ± 1 g, de verre soluble 25 g ± 1 g et d'eau déminéralisée 300 ml ± 1 ml dans le malaxeur Hollander et agitation afin d'obtenir l'agent de revêtement se présentant sous forme de liquide visqueux, la vitesse d'agitation étant de 50r/min, le temps d'agitation de 80 min ;(3) pré-traitement des particules de carbure de bore① broyage à billes : pesée de carbure de bore 300 g ± 0,1 g, mis en place dans le réservoir du broyeur à billes, et soumis à un broyage à billes afin d'obtenir une poudre fine ayant une granulométrie ≤ 9 µm, la vitesse de broyage à billes speed étant de 80r/min, le temps de broyage à billes de 3 h ;② lavage à dispersion ultrasonique : après le broyage à billes, versement de la poudre fine dans un bécher et ajout d'alcool pur 500 ml ± 1 ml, mélange ;
mise en place du bécher dans un disperseur ultrasonique et exécution du lavage à dispersion ultrasonique afin d'obtenir le liquide de mélange, la fréquence ultrasonore étant de 60 kHz et le temps de dispersion ultrasonique de 80 min ;③ filtration : versement du liquide de mélange dans la cheminée de tissu de la bouteille filtrante, filtration par membrane microporeuse, retrait du surnageant, et conservation du gâteau de filtration ;④ traitement de séchage et d'oxydation : mise en place du gâteau de filtration dans le four de traitement thermique, application du traitement de séchage et d'oxydation à haute température, obtention de la poudre fine de carbure de bore après séchage, la température de séchage et d'oxydation étant de 500 °C et le temps de séchage et d'oxydation de 2 h ;(4) pré-traitement du magnésium, du zinc et de l'alliage magnésium-yttrium et du moule de coulée sous pression de type fermé-ouvert① découpe mécanique en pièces du magnésium, du zinc et de l'alliage magnésium-yttrium, la grandeur de pièce étant ≤ 30 mm × 30 mm × 10 mm ;② lavage de surface par alcool pur du magnésium, du zinc et de l'alliage magnésium-yttrium et mise en place dans le four de séchage sous vide après lavage, la température de séchage étant de 100 °C, le degré de vide de 2 Pa et la durée de séchage de 30 min ;③ emballage du carbure de bore avec du papier d'aluminium, mise en place dans le four de séchage sous vide et séchage, la température de séchage étant de 100 °C, le degré de vide de 2 Pa et la durée de séchage de 60 min ;
pré-chauffage du moule de coulée sous pression de type fermé-ouvert et revêtement de la surface intérieure de la cavité de moule par l'agent de revêtement préparé, l'épaisseur de l'agent de revêtement étant de1mm ; à l'issue du revêtement, mise en place du moule de coulée sous pression de type fermé-ouvert dans le four de chauffage et pré-chauffage, la température de pré-chauffage étant de 150 °C et le temps de pré-chauffage de 1 h ;(5) fusion de l'alliage de magnésium
la fusion de l'alliage de magnésium est exécutée dans le four de fusion par induction à fréquence moyenne sous vide et terminée par processus de chauffage par induction à fréquence moyenne, mise sous vide, soufflage d'argon par le fond et agitation mécanique,① ouverture du four de fusion par induction à fréquence moyenne sous vide et nettoyage de la partie intérieure du creuset de fusion en graphite pour rendre propre la partie intérieure du creuset ;② pesée d'un bloc de magnésium de 4127 g ± 0,1 g, d'un bloc de zinc de 784 g ± 0,1 g et d'un bloc d'alliage magnésium-yttrium de 571 g ± 0,1 g, et mise en place de ceux-ci au fond du creuset ;③ fermeture du four de fusion par induction à fréquence moyenne sous vide et verrouillage de celui-ci ;
activation de la pompe à vide et extraction de l'air intérieur pour que la pression à l'intérieur du atteigne 1 Pa ;
activation du chauffage du four de fusion par induction à fréquence moyenne pour commencer le chauffage, la température de chauffage étant de 610 °C ± 1 °C ;④ activation du dispositif de soufflage d'argon par le fond pour alimenter le creuset en argon, la vitesse de soufflage d'argon par le fond étant de 200cm3/min ; réglage de la pression à l'intérieur du four pour porter à un bar la pression à l'intérieur du four et régulation par la vanne de sortie ;⑤ si la température de fusion est de 610 °C ± 1 °C, ajout de poudre fine de carbure de bore par le dispositif d'alimentation à vide ; activation de l'agitateur mécanique, la vitesse d'aspiration étant de 20r/min et le temps d'agitation de 10 min ;⑥ arrêt de l'agitation et poursuite du chauffage ; si la température de fusion atteint 730 °C ± 1 °C, désactivation de l'agitateur mécanique et du conduit de soufflage d'argon par le fond, durée de repos 10 min et préparation pour la coulée ;(6) coulée sous pression① ouverture du four de fusion par induction à fréquence moyenne sous vide, retrait des scories à la surface de la fonte dans le creuset, coulée de l'alliage fondu dans la cavité du moule de coulée sous pression ; activation de la machine à couler sous pression et compression du métal fondu par le poinçon, la pression étant de 250 MPa et le temps de maintien de 20 s ;
la réaction d'alliage survenant pendant la solidification des quasi-cristaux Mg-Zn-Y estune phase quasi-cristalline Mg3Zn6Y stable pouvant être obtenue, la formule de réaction étantα-Mg: phase de substrat magnésiumMg3Zn6Y : phase quasi-cristalline magnésium-zinc-yttrium② éjection du moulage et refroidissement à l'air à 25 °C pour produire les quasi-cristaux magnésium-zinc-yttrium et les blocs de matériau composite à base de Mg renforcés par mélange de carbure de bore ;(7) traitement thermique du moulage① chargement pour traitement thermique des quasi-cristaux magnésium-zinc-yttrium et des blocs de matériau composite à base de Mg renforcés par mélange de carbure de bore dans le four de traitement thermique sous vide, la température du traitement thermique étant de 420 °C, le degré de vide de 2 Pa, et le temps de traitement thermique de 15 h ; puis trempage rapide du moulage dans l'eau chaude à 50 °C, traitement de trempe, le temps de trempe étant de 20 s ;② mise en place du moulage dans le four de traitement thermique après trempe pour traitement de vieillissement à 200 °C pendant 8 h ; puis arrêt du chauffage et refroidissement à 25 °C dans le four de traitement thermique ;(8) nettoyage, détection, analyse et caractérisation
nettoyage de la surface du moulage pour le rendre propre ; détection, analyse et caractérisation de la microstructure et des propriétés mécaniques ;
analyse de la structure métallographique avec un microscope optique ;
essai de résistance à la traction et de dureté avec une machine d'essai de traction universelle et un testeur de dureté ;
analyse de morphologie de fracture avec un microscope électronique à balayage ; analyse XRD avec un diffractomètre à rayon X ;
conclusion : les quasi-cristaux magnésium-zinc-yttrium et les matériaux composites à base de Mg renforcés par mélange de carbure de bore sont des blocs rectangulaires, la résistance à la traction étant de 315 MPa, l'allongement de 7 %, la dureté atteignant 108 Hv. - Procédé de préparation de matériaux composites à base de Mg renforcés par mélange de quasi-cristaux magnésium-zinc-yttrium et de carbure de bore selon la revendication 1, caractérisé en ce que la fusion des matériaux composites à base de Mg est exécutée dans le four de fusion par induction à fréquence moyenne sous vide et terminée par processus de chauffage par induction à fréquence moyenne, soufflage d'argon par le fond et agitation mécanique ;
le four de fusion par induction à fréquence moyenne sous vide est un four vertical ;
le fond du four de fusion par induction à fréquence moyenne sous vide (1) est prévu avec une base de four (2), et à l'intérieur du four de fusion par induction à fréquence moyenne sous vide (1), une chambre de four (3) ; une table de travail (6) est prévue au fond de la chambre de four (3) et un creuset de fusion en graphite (7) est disposé sur la table de travail (6) ; l'extérieur du creuset de fusion en graphite (7) est entouré par le chauffage par induction à fréquence moyenne (8) et l'intérieur du creuset de fusion en graphite (7) contient l'alliage fondu (9) ; un conduit de sortie (4) est prévu en haut à droite du four de fusion par induction à fréquence moyenne sous vide (1) et est commandé par la vanne de sortie (5) ; la bouteille d'argon (15) est prévue en haut à gauche du four de fusion par induction à fréquence moyenne sous vide (1) et un conduit d'argon (16) ainsi qu'une vanne à argon (17) sont prévus sur la bouteille d'argon (15) ; le conduit d'argon (16) est relié au moteur de soufflage par le fond (11) ; le moteur de soufflage par le fond (11) est relié au conduit de soufflage par le fond (12) ; le conduit de soufflage par le fond (12) communique avec le creuset de fusion en graphite (7) en traversant la base de four (2) et la table de travail (6), et souffle par le fond l'alliage fondu (9) ; une pompe à vide (13est prévue en bas à droite de la base de four (2) et communique avec la chambre de four (3) par un conduit de vide (14) ; un conduit d'alimentation (27), une vanne d'alimentation (28) et un agitateur mécanique (29) sont prévus sur le dessus du four de fusion par induction à fréquence moyenne sous vide (1), et le conduit d'alimentation (27) et l'agitateur mécanique (29) s'étendent vers le creuset de fusion en graphite (7) en traversant la base supérieure du four ;
une armoire électrique (18) est prévue à droite du four de fusion par induction à fréquence moyenne sous vide (1) et un écran d'affichage (19), un voyant indicateur (20), un interrupteur (21), un dispositif de commande (22) du chauffage par induction à fréquence moyenne, un dispositif de commande (23) du moteur de soufflage par le fond et un dispositif de commande (24) de la pompe à vide sont prévus sur l'armoire électrique (18) ; l'armoire électrique (18) est reliée au chauffage par induction à fréquence moyenne (8) par un premier câble (25) ; l'armoire électrique (18) est reliée au moteur de soufflage par le fond (11) et à une pompe à vide (13) par le deuxième câble (26) ; la cavité du four (3) est remplie d'argon (10).
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CN111842852A (zh) * | 2020-07-30 | 2020-10-30 | 兰州理工大学 | 液模锻浸渗制备耐磨耐蚀高强度铜及铜合金结构件的方法 |
CN113106277B (zh) * | 2021-04-10 | 2022-03-01 | 中北大学 | 一种镁锌钇准晶和碳化钛协同强化镁基复合材料的制备方法 |
CN113798494A (zh) * | 2021-08-12 | 2021-12-17 | 山东科技大学 | 一种TiB2颗粒增强镁基复合材料及其制备方法 |
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