CN103667840A - Nanoparticle reinforced polybasic heat-insulating magnesium alloy and preparation method thereof - Google Patents
Nanoparticle reinforced polybasic heat-insulating magnesium alloy and preparation method thereof Download PDFInfo
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 55
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000956 alloy Substances 0.000 claims abstract description 104
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 98
- 239000011777 magnesium Substances 0.000 claims abstract description 24
- 229910052718 tin Inorganic materials 0.000 claims abstract description 18
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 18
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 9
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 9
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 8
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims description 40
- 238000007670 refining Methods 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000000137 annealing Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 20
- 238000005096 rolling process Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 238000003723 Smelting Methods 0.000 claims description 15
- 230000002787 reinforcement Effects 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 229910018131 Al-Mn Inorganic materials 0.000 claims description 10
- 229910018167 Al—Be Inorganic materials 0.000 claims description 10
- 229910018182 Al—Cu Inorganic materials 0.000 claims description 10
- 229910018461 Al—Mn Inorganic materials 0.000 claims description 10
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000008187 granular material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 10
- 239000000155 melt Substances 0.000 claims description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 238000005275 alloying Methods 0.000 claims description 5
- 239000000470 constituent Substances 0.000 claims description 5
- 229910001610 cryolite Inorganic materials 0.000 claims description 5
- 238000005242 forging Methods 0.000 claims description 5
- -1 fully stir Substances 0.000 claims description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 238000007669 thermal treatment Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000009736 wetting Methods 0.000 claims description 5
- 229910001339 C alloy Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910018125 Al-Si Inorganic materials 0.000 description 2
- 229910018520 Al—Si Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229910018140 Al-Sn Inorganic materials 0.000 description 1
- 229910018564 Al—Sn Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910007570 Zn-Al Inorganic materials 0.000 description 1
- 229910007610 Zn—Sn Inorganic materials 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Abstract
The invention provides a nanoparticle reinforced polybasic heat-insulating magnesium alloy, which contains the following components in percentage by weight: 0.5-0.7 percent of Gd, 3.35-3.6 percent of Al, 1.7-1.95 percent of Zn, 0.9-1.0 percent of Ca, 1.0-1.1 percent of Sr, 0.8-1.0 percent of Nd, 0.1-0.3 percent of Zr, 1-2 percent of Sn, 0.15-0.20 percent of Be, 0.7-1.0 percent of Mn, 0.1-0.15 percent of Sb, 0.5-0.8 percent of Cu, 4-10 percent of SiC nanoparticles and the balance of Mg, wherein the diameters of the SiC nanoparticles are less than 100 nanometers. The invention further provides a preparation method of the alloy. The alloy has high mechanical property and high creep resistance.
Description
Technical field
The invention belongs to heatproof magnesium alloy material field, especially a kind of nano-particle reinforcement multicomponent heat-resistant magnesium alloy and preparation method thereof.
Background technology
Magnesium alloy is as the commercial metal engineering structured material of lightweight, because it has that light specific gravity, specific tenacity specific rigidity are high, damping vibration attenuation falls that dry ability is strong, liquid condition shaping superior performance and be easy to the advantages such as recycling, is described as 21 century " green structured material ".But at present because the high-temperature creep resistance of existing magnesium alloy is poor, long term operation temperature can not be over 120 ℃, make it for the manufacture of to the high motor car engine of high temperature creep property requirement and other drive disk assemblies, therefore greatly hinder the further application of magnesium alloy.Also just because of like this, for the research and development with the heat resistance magnesium alloy of high-temperature creep resistance, given great attention both at home and abroad, and the heat resistance magnesium alloy of the series such as Mg-Al-Si, Mg-Al-RE, Mg-Al-Ca, Mg-Al-Ca-RE, Mg-Al-Sr, Mg-Al-Sn, Mg-Zn-Al, Mg-Zn-RE, Mg-Zn-Si, Mg-Zn-Sn, Mg-Y-Nd and Mg-Sn-Ca has been studied in successively trial-production.Yet, these obtain in the heat resistance magnesium alloy system of trial-production research in the above, really obtain mainly concentrating on minority alloy of practical application, as AS41 and the AS21 alloy of the WE43 alloy of the AE42 alloy in Mg-Al-RE system, Mg-Y-Nd system and Mg-Al-Si system.In addition, even if these heat resistance magnesium alloys that are applied also make its application be subject to restriction in various degree because there is different separately problems.As for AE42 alloy and WE43 alloy, it all contains RE (> 2.5%) and/or the precious metal element such as Y, Th of high-content, the cost of alloy is higher, and it is at present only for the contour performance engine of racing car, not widespread use on automobile.Therefore, be necessary the further novel heat resistance magnesium alloy of research and development.
At current particle, strengthen in cast magnesium alloys technique and technology, mostly adopt micron particles reinforcement, the plasticity of sacrificial magnesium alloy material of take obtains the raising (D.J.Lioyd of intensity to a certain extent as cost, International Materials Reviews, 1994, Vol 39).And nano material has special performance and the study hotspot that becomes, the magnesium alloy materials that adopts nanometer reinforcement to strengthen is expected to integrate nano material and matrix material, and material property is further improved.The method of using mechanical alloying to prepare reinforced by nanoparticles magnesium base composite material is applicable to the preparation (H.Ferkel etc. of reinforced by nanoparticles deformed magnesium alloy material, Materials Science and Engineering A, 2001, Vol 298), utilize ultrasonic technology to prepare reinforced by nanoparticles magnesium alloy materials and also have certain effect (Jie Lan etc., Materials Science and Engineering A, 2004, Vol 386), but above method all has complex process, equipment requirements is high, preparation is little in batches, the restriction that cost is high, be not suitable for preparation and the forming technology of reinforced by nanoparticles casting magnesium alloy material.
Summary of the invention
The object of the present invention is to provide a kind of nano-particle reinforcement multicomponent heat-resistant magnesium alloy and preparation method thereof.
For reaching this object, the present invention by the following technical solutions:
A nano-particle reinforcement multicomponent heat-resistant magnesium alloy, is characterized in that, according to weight percent content, contains: Gd:0.5-0.7%, Al:3.35-3.6%, Zn:1.7-1.95%, Ca:0.9-1.0%, Sr:1.0-1.1%, Nd:0.8-1.0%, Zr:0.1-0.3%, Sn:1-2%, Be:0.15-0.20%, Mn:0.7-1.0%, Sb:0.1-0.15%, Cu:0.5-0.8%, SiC nano particle: 4-10%, surplus is Mg, and the diameter of SiC nano particle is less than 100nm.
The preparation method of described nano-particle reinforcement multicomponent heat-resistant magnesium alloy, it comprises the following steps:
(1) raw material is prepared: according to weight percent content, carry out raw material preparation, described raw material is pure Mg ingot, Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy;
Nano SiC granule pre-treatment: a, in container, pour appropriate analytical pure ethanol into, a certain amount of dry SiC nano particle is put into container, stir, fully wetting, the ratio of SiC particle and ethanol is 1-5g:3-50ml; B, the polyvinyl alcohol dilute solution that accounts for said mixture volume 1/50～1/10 is added in the mixture of SiC particle and ethanol, fully stir, mix; C, the said mixture that contains SiC nano particle is placed in to baking oven toasts, dry, storing temperature is 80～95 ℃.
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 745-770 ℃, first in smelting furnace, add pure Mg ingot, after pure magnesium ingot melts completely, add Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy, after melting completely, stir all raw materials, make alloying constituent even, then add pretreated nano SiC granule, stir again, it is mixed,
(3) refining: make smelting furnace be warming up to 785 ℃～800 ℃ alloys and carry out refining, add while stirring heat resistance magnesium alloy refining agent, refining time is 1-4 minute, after refining is complete standing 5～8 minutes of 740 ℃～750 ℃ insulations, the consisting of of described heat resistance magnesium alloy refining agent: NaCl:11%～15%; Na3AlF6:8～10%; MgCl2:30-40%; Surplus is KCl;
(4) casting: it is that in the swage tool of 200～300 ℃, pouring temperature is 730 ℃～740 ℃ that the magnesium alloy refining material of melting is cast to preheating temperature; Foundry goods specification is Ф 450mm～Ф 500mm, length >=3000mm
(5) thermal treatment: foundry goods is carried out to solution treatment in 435-440 ℃ of temperature range, and the solution treatment time is 16～24 hours, then carries out shrend, puts into the foundry goods after quenching in the resistance furnace of 210 ℃ artificial aging 40 hours, makes magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 410 ℃～450 ℃ insulation 1～2h; Carry out two to hammer cogging, be forged into the slab that thickness is 40-60mm; Reduction in pass is 20%～40%, and every 3-6 passage is forged after annealing 1.5h, and annealing temperature is 410 ℃～450 ℃; B. heated roll to temperature is 310-350 ℃; C. heating slab to temperature is 460-470 ℃, is incubated after 20-30 minute, adopts the method for multi-pass small deformation amount that heavy plate rolling is become to 2～10mm thin plate, and the speed of rolls is 0.4m/s～0.8 m/s; Every time rolling draught is 10%～20%, after every time rolling, melts down annealing, and annealing temperature is 410 ℃～450 ℃, and annealing time is 30min～40min;
(7) roll postheat treatment: the thin plate after rolling is carried out to ageing treatment, and described aging treatment process is: aging temp is 230-250 ℃, soaking time is 12-36h; At 200-220 ℃, carry out ageing treatment for the second time again, aging time is 12-36h; Finally at 150-180 ℃, carry out ageing treatment for the third time, aging time is 12-36h.
Further, according to weight percent content, contain: Gd:0.65%, Al:3.55%, Zn:1.85%, Ca:0.96%, Sr:1.05%, Nd:0.9%, Zr:0.24%, Sn:1.6%, Be:0.18%, Mn:0.85%, Sb:0.13%, Cu:0.75%, SiC nano particle: 4.5%, surplus is Mg, the diameter of SiC nano particle is 50nm.
The invention has the advantages that:
1,, on the basis of complex magnesium alloy, by adding nano reinforcement particle, improve the obdurability of magnesium alloy;
2, developed new nano particle pretreatment technology, made nano particle more effective adding in magnesium alloy;
3, nano-particle reinforcement multicomponent heat-resistant magnesium alloy of the present invention has excellent mechanical performances and creep-resistant property.
Embodiment
embodiment 1
A nano-particle reinforcement multicomponent heat-resistant magnesium alloy, contains according to weight percent content: Gd:0.55%, Al:3.4%, Zn:1.75%, Ca:0.93%, Sr:1.02%, Nd:0.88%, Zr:0.17%, Sn:1.6%, Be:0.18%, Mn:0.76%, Sb:0.13%, Cu:0.59%, SiC nano particle: 5%, surplus is Mg; The diameter of SiC nano particle is less than 90nm, and the preparation method of described heat resistance magnesium alloy, comprises the following steps:
(1) raw material is prepared: according to weight percent content, carry out raw material preparation, described raw material is pure Mg ingot, Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy;
Nano SiC granule pre-treatment: a, in container, pour appropriate analytical pure ethanol into, a certain amount of dry SiC nano particle is put into container, stir, fully wetting, the ratio of SiC particle and ethanol is 2g:10ml; B, the polyvinyl alcohol dilute solution that accounts for said mixture volume 1/40 is added in the mixture of SiC particle and ethanol, fully stir, mix; C, the said mixture that contains SiC nano particle is placed in to baking oven toasts, dry, storing temperature is 90 ℃;
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 750 ℃, first in smelting furnace, add pure Mg ingot, after pure magnesium ingot melts completely, add Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy, after all raw materials melt completely, stir, make alloying constituent even; Then add pretreated nano SiC granule, then stir, it is mixed;
(3) refining: make smelting furnace be warming up to 790 ℃ of alloys and carry out refining, add while stirring heat resistance magnesium alloy refining agent, refining time is 4 minutes, after refining is complete standing 6 minutes of 745 ℃ of insulations, the consisting of of described heat resistance magnesium alloy refining agent: NaCl:13%; Na3AlF6:9%; MgCl2:35%; Surplus is KCl;
(4) casting: it is that in the swage tool of 260 ℃, pouring temperature is 735 ℃ that the magnesium alloy refining material of melting is cast to preheating temperature; Foundry goods specification is Ф 45, length 3000mm
(5) thermal treatment: foundry goods is carried out to solution treatment in 435 ℃ of temperature ranges, and the solution treatment time is 24 hours, then carries out shrend, puts into the foundry goods after quenching in the resistance furnace of 210 ℃ artificial aging 40 hours, makes magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 410 ℃ of insulation 2h; Carry out two to hammer cogging, be forged into the slab that thickness is 60mm; Reduction in pass is 35%, and every 4 passages are forged after annealing 1.5h, and annealing temperature is 410 ℃; B. heated roll to temperature is 350 ℃; C. heating slab to temperature is 470 ℃, is incubated after 30 minutes, adopts the method for multi-pass small deformation amount that heavy plate rolling is become to 3mm thin plate, and the speed of rolls is 0.7 m/s; Every time rolling draught is 15%, after every time rolling, melts down annealing, and annealing temperature is 4100 ℃, and annealing time is 35min;
(7) roll postheat treatment: the thin plate after rolling is carried out to ageing treatment, and described aging treatment process is: aging temp is 245 ℃, soaking time is 16h; At 215 ℃, carry out ageing treatment for the second time again, aging time is 16h; Finally at 165 ℃, carry out ageing treatment for the third time, aging time is 16h.
embodiment 2:
A nano-particle reinforcement multicomponent heat-resistant magnesium alloy, contains according to weight percent content: Gd:0.68%, Al:3.54%, Zn:1.82%, Ca:0.96%, Sr:1.07%, Nd:0.98%, Zr:0.23%, Sn:1.7%, Be:0.175%, Mn:0.89%, Sb:0.145%, Cu:0.67%, SiC nano particle: 5.5%, surplus is Mg; The diameter of SiC nano particle is less than 20nm;
The preparation method of described heat resistance magnesium alloy, comprises the following steps:
(1) raw material is prepared: according to weight percent content, carry out raw material preparation, described raw material is pure Mg ingot, Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy;
Nano SiC granule pre-treatment: a, in container, pour appropriate analytical pure ethanol into, a certain amount of dry SiC nano particle is put into container, stir, fully wetting, the ratio of SiC particle and ethanol is 5g:20ml; B, the polyvinyl alcohol dilute solution that accounts for said mixture volume 1/30 is added in the mixture of SiC particle and ethanol, fully stir, mix; C, the said mixture that contains SiC nano particle is placed in to baking oven toasts, dry, storing temperature is 85 ℃;
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 745-770 ℃, first in smelting furnace, add pure Mg ingot, after pure magnesium ingot melts completely, add Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy, after all raw materials melt completely, stir, make alloying constituent even; Then add pretreated nano SiC granule, then stir, it is mixed;
(3) refining: make smelting furnace be warming up to 790 ℃ of alloys and carry out refining, add while stirring heat resistance magnesium alloy refining agent, refining time is 4 minutes, after refining is complete standing 8 minutes of 740 ℃ of insulations, the consisting of of described heat resistance magnesium alloy refining agent: NaCl:13%; Na3AlF6:9%; MgCl2:36%; Surplus is KCl;
(4) casting: it is that in the swage tool of 240 ℃, pouring temperature is 38 ℃ that the magnesium alloy refining material of melting is cast to preheating temperature; Foundry goods specification is Ф 480mm, length 3500mm
(5) thermal treatment: foundry goods is carried out to solution treatment in 440 ℃ of temperature ranges, and the solution treatment time is 16 hours, then carries out shrend, puts into the foundry goods after quenching in the resistance furnace of 210 ℃ artificial aging 40 hours, makes magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 435 ℃ of insulation 1.5h; Carry out two to hammer cogging, be forged into the slab that thickness is 45mm; Reduction in pass is 25%, and every 3 passages are forged after annealing 1.5h, and annealing temperature is 430 ℃; B. heated roll to temperature is 320 ℃; C. heating slab to temperature is 465 ℃, is incubated after 25 minutes, adopts the method for multi-pass small deformation amount that heavy plate rolling is become to 4mm thin plate, and the speed of rolls is 0.45 m/s; Every time rolling draught is 12%, after every time rolling, melts down annealing, and annealing temperature is 435 ℃, and annealing time is 35min;
(7) roll postheat treatment: the thin plate after rolling is carried out to ageing treatment, and described aging treatment process is: aging temp is 250 ℃, soaking time is 12h; At 220 ℃, carry out ageing treatment for the second time again, aging time is 12h; Finally at 180 ℃, carry out ageing treatment for the third time, aging time is 12h.
embodiment 3:
A nano-particle reinforcement multicomponent heat-resistant magnesium alloy, contains Gd:0.65% according to weight percent content, Al:3.55%, Zn:1.85%, Ca:0.96%, Sr:1.05%, Nd:0.9%, Zr:0.24%, Sn:1.6%, Be:0.18%, Mn:0.85%, Sb:0.13%, Cu:0.75%, SiC nano particle: 8%, surplus is Mg, the diameter of SiC nano particle is 25nm.
The preparation method of described heat resistance magnesium alloy, comprises the following steps:
(1) raw material is prepared: according to weight percent content, carry out raw material preparation, described raw material is pure Mg ingot, Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy;
Nano SiC granule pre-treatment: a, in container, pour appropriate analytical pure ethanol into, a certain amount of dry SiC nano particle is put into container, stir, fully wetting, the ratio of SiC particle and ethanol is 3g:10ml; B, the polyvinyl alcohol dilute solution that accounts for said mixture volume 1/25 is added in the mixture of SiC particle and ethanol, fully stir, mix; C, the said mixture that contains SiC nano particle is placed in to baking oven toasts, dry, storing temperature is 92 ℃;
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 750 ℃, first in smelting furnace, add pure Mg ingot, after pure magnesium ingot melts completely, add Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy, after all raw materials melt completely, stir, make alloying constituent even; Then add pretreated nano SiC granule, then stir, it is mixed;
(3) refining: make smelting furnace be warming up to 790 ℃ of alloys and carry out refining, add while stirring heat resistance magnesium alloy refining agent, refining time is 4 minutes, after refining is complete standing 8 minutes of 740 ℃ of insulations, the consisting of of described heat resistance magnesium alloy refining agent: NaCl:13%; Na3AlF6:9%; MgCl2:36%; Surplus is KCl;
(4) casting: it is that in the swage tool of 240 ℃, pouring temperature is 38 ℃ that the magnesium alloy refining material of melting is cast to preheating temperature; Foundry goods specification is Ф 480mm, length 3500mm
(5) thermal treatment: foundry goods is carried out to solution treatment in 440 ℃ of temperature ranges, and the solution treatment time is 16 hours, then carries out shrend, puts into the foundry goods after quenching in the resistance furnace of 210 ℃ artificial aging 40 hours, makes magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 435 ℃ of insulation 1.5h; Carry out two to hammer cogging, be forged into the slab that thickness is 45mm; Reduction in pass is 25%, and every 3 passages are forged after annealing 1.5h, and annealing temperature is 430 ℃; B. heated roll to temperature is 320 ℃; C. heating slab to temperature is 465 ℃, is incubated after 25 minutes, adopts the method for multi-pass small deformation amount that heavy plate rolling is become to 4mm thin plate, and the speed of rolls is 0.45 m/s; Every time rolling draught is 12%, after every time rolling, melts down annealing, and annealing temperature is 435 ℃, and annealing time is 35min;
(7) roll postheat treatment: the thin plate after rolling is carried out to ageing treatment, and described aging treatment process is: aging temp is 250 ℃, soaking time is 12h; At 220 ℃, carry out ageing treatment for the second time again, aging time is 12h; Finally at 180 ℃, carry out ageing treatment for the third time, aging time is 12h.
the performance of the alloy that embodiment 1-3 obtains is listed in the table below
Claims (3)
1. a nano-particle reinforcement multicomponent heat-resistant magnesium alloy, is characterized in that: according to weight percent content, contain: Gd:0.5-0.7%, Al:3.35-3.6%, Zn:1.7-1.95%, Ca:0.9-1.0%, Sr:1.0-1.1%, Nd:0.8-1.0%, Zr:0.1-0.3%, Sn:1-2%, Be:0.15-0.20%, Mn:0.7-1.0%, Sb:0.1-0.15%, Cu:0.5-0.8%, SiC nano particle: 4-10%, surplus is Mg, the diameter of SiC nano particle is less than 100nm.
2. the preparation method of a kind of nano-particle reinforcement multicomponent heat-resistant magnesium alloy as claimed in claim 1, is characterized in that:
(1) raw material is prepared: according to weight percent content, carry out raw material preparation, described raw material is pure Mg ingot, Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy;
Nano SiC granule pre-treatment: a, in container, pour appropriate analytical pure ethanol into, a certain amount of dry SiC nano particle is put into container, stir, fully wetting, the ratio of SiC particle and ethanol is 1-5g:3-50ml; B, the polyvinyl alcohol dilute solution that accounts for said mixture volume 1/50～1/10 is added in the mixture of SiC particle and ethanol, fully stir, mix; C, the said mixture that contains SiC nano particle is placed in to baking oven toasts, dry, storing temperature is 80～95 ℃;
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 745-770 ℃, first in smelting furnace, add pure Mg ingot, after pure magnesium ingot melts completely, add Mg-Gd master alloy, pure Al ingot, pure Zn, Al-Ca master alloy, Al-Sr master alloy, Mg-Nd master alloy, Mg-Zr master alloy, pure Sn, Al-Be master alloy, Al-Mn master alloy, pure Sb, Al-Cu master alloy, after melting completely, stir all raw materials, make alloying constituent even, then add pretreated nano SiC granule, stir again, it is mixed,
(3) refining: make smelting furnace be warming up to 785 ℃～800 ℃ alloys and carry out refining, add while stirring heat resistance magnesium alloy refining agent, refining time is 1-4 minute, after refining is complete standing 5～8 minutes of 740 ℃～750 ℃ insulations, the consisting of of described heat resistance magnesium alloy refining agent: NaCl:11%～15%; Na3AlF6:8～10%; MgCl2:30-40%; Surplus is KCl;
(4) casting: it is that in the swage tool of 200～300 ℃, pouring temperature is 730 ℃～740 ℃ that the magnesium alloy refining material of melting is cast to preheating temperature; Foundry goods specification is Ф 450mm～Ф 500mm, length >=3000mm
(5) thermal treatment: foundry goods is carried out to solution treatment in 435-440 ℃ of temperature range, and the solution treatment time is 16～24 hours, then carries out shrend, puts into the foundry goods after quenching in the resistance furnace of 210 ℃ artificial aging 40 hours, makes magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 410 ℃～450 ℃ insulation 1～2h; Carry out two to hammer cogging, be forged into the slab that thickness is 40-60mm; Reduction in pass is 20%～40%, and every 3-6 passage is forged after annealing 1.5h, and annealing temperature is 410 ℃～450 ℃; B. heated roll to temperature is 310-350 ℃; C. heating slab to temperature is 460-470 ℃, is incubated after 20-30 minute, adopts the method for multi-pass small deformation amount that heavy plate rolling is become to 2～10mm thin plate, and the speed of rolls is 0.4m/s～0.8 m/s; Every time rolling draught is 10%～20%, after every time rolling, melts down annealing, and annealing temperature is 410 ℃～450 ℃, and annealing time is 30min～40min;
(7) roll postheat treatment: the thin plate after rolling is carried out to ageing treatment, and described aging treatment process is: aging temp is 230-250 ℃, soaking time is 12-36h; At 200-220 ℃, carry out ageing treatment for the second time again, aging time is 12-36h; Finally at 150-180 ℃, carry out ageing treatment for the third time, aging time is 12-36h.
3. the preparation method of the nano-particle reinforcement multicomponent heat-resistant magnesium alloy as described in claim 1-2, is characterized in that: according to weight percent content, contain: Gd:0.65%, Al:3.55%, Zn:1.85%, Ca:0.96%, Sr:1.05%, Nd:0.9%, Zr:0.24%, Sn:1.6%, Be:0.18%, Mn:0.85%, Sb:0.13%, Cu:0.75%, SiC nano particle: 4.5%, surplus is Mg, the diameter of SiC nano particle is 50nm.
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| CN104099506A (en) * | 2014-08-06 | 2014-10-15 | 杨攀 | Multicomponent heat-resistant magnesium alloy and production method thereof |
| CN104313441A (en) * | 2014-11-03 | 2015-01-28 | 北京汽车股份有限公司 | High-modulus rare earth magnesium-based composite material containing SiC particles |
| CN104630588A (en) * | 2015-01-04 | 2015-05-20 | 河南科技大学 | Magnesium-based composite material and composite cookware |
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| CN105369094A (en) * | 2014-08-25 | 2016-03-02 | 武汉赛润科技有限公司 | Nano-particle reinforced magnesium alloy |
| CN105369094B (en) * | 2014-08-25 | 2018-01-02 | 浙江博来工具有限公司 | A kind of nano-particle reinforcement magnesium alloy |
| CN104313441B (en) * | 2014-11-03 | 2018-01-16 | 北京汽车股份有限公司 | A kind of rare earth and magnesium-based composite of high-modulus containing SiC particulate |
| CN104313441A (en) * | 2014-11-03 | 2015-01-28 | 北京汽车股份有限公司 | High-modulus rare earth magnesium-based composite material containing SiC particles |
| CN104630588A (en) * | 2015-01-04 | 2015-05-20 | 河南科技大学 | Magnesium-based composite material and composite cookware |
| WO2016179734A1 (en) * | 2015-05-12 | 2016-11-17 | 苏州列治埃盟新材料技术转移有限公司 | Magnesium-aluminum-silicon carbide intermediate alloy material and preparation method therefor |
| CN105463281A (en) * | 2016-01-15 | 2016-04-06 | 佛山市领卓科技有限公司 | High-strength light metal and preparation method thereof |
| CN105525109A (en) * | 2016-01-15 | 2016-04-27 | 佛山市领卓科技有限公司 | Silicon carbide strengthened magnesium alloy and preparing method thereof |
| CN105624502A (en) * | 2016-01-15 | 2016-06-01 | 佛山市领卓科技有限公司 | Ultrahigh-modulus magnesium alloy and preparation method thereof |
| CN105463281B (en) * | 2016-01-15 | 2018-02-09 | 佛山市领卓科技有限公司 | A kind of high-strength light metal and preparation method thereof |
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| CN105525109B (en) * | 2016-01-15 | 2018-06-08 | 佛山市领卓科技有限公司 | A kind of SiC reinforcement magnesium alloy and preparation method thereof |
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