CN103667840B - A kind of nano-particle reinforcement multicomponent heat-resistant magnesium alloy and preparation method thereof - Google Patents
A kind of nano-particle reinforcement multicomponent heat-resistant 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
- 230000002787 reinforcement Effects 0.000 title claims abstract description 17
- 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
- 239000000203 mixture Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 238000003723 Smelting Methods 0.000 claims description 15
- 238000005096 rolling process Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 13
- 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
- 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
- 238000005242 forging Methods 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
- 239000000463 material Substances 0.000 claims description 10
- 239000000155 melt Substances 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 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
- -1 fully stir Substances 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
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 229910001610 cryolite Inorganic materials 0.000 description 4
- 229910001629 magnesium chloride Inorganic materials 0.000 description 4
- 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
- 238000005266 casting Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate 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
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Abstract
The invention provides a kind of nano-particle reinforcement multicomponent heat-resistant magnesium alloy, contain according to weight percent content: 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 that the diameter of Mg, SiC nano particle is less than 100nm.The present invention also proposes the preparation method of this alloy.This alloy has excellent mechanical performances and creep-resistant property.
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 as the commercial metal structural timber of most lightweight, because of its have 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 service temperature can not more than 120 DEG C, it is made for the manufacture of to the high motor car engine of high temperature creep property requirement and other drive disk assemblies, therefore cannot greatly to hinder the further application of magnesium alloy.Also just because of like this, research and development both at home and abroad for the heat resistance magnesium alloy with high-temperature creep resistance give great attention, and successively trial-production have studied 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.But, above, these obtain manufacturing experimently in the heat resistance magnesium alloy system of research, what really obtain practical application mainly concentrates on minority alloy, as the WE43 alloy of the AE42 alloy in Mg-Al-RE system, Mg-Y-Nd system and AS41 and the AS21 alloy of Mg-Al-Si system.In addition, even if these heat resistance magnesium alloys be applied also make it apply to be subject to restriction in various degree because there is problems different separately.As for AE42 alloy and WE43 alloy, its precious metal element such as RE (> 2.5%) and/or Y, Th all containing 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, the heat resistance magnesium alloy that research and development are novel is further necessary.
In current particle reinforce cast magnesium alloys technique and technology, most employing micron particles reinforcement, with the plasticity of sacrificial magnesium alloy material for cost obtains the raising (D.J.Lioyd of intensity to a certain extent, International Materials Reviews, 1994, Vol 39).And the study hotspot that nano material has special performance and becomes, the magnesium alloy materials adopting nanometer reinforcement to strengthen is expected to integrate nano material and matrix material, and material property is further improved.The method 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 batch is little, 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 kind of nano-particle reinforcement multicomponent heat-resistant magnesium alloy, is characterized in that, contain according to weight percent content: 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 that the diameter of Mg, 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 prepares: carry out raw material preparation according to weight percent content, 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, pour appropriate analytical pure ethanol in a reservoir, 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 accounting for said mixture volume 1/50 ~ 1/10 to be added in the mixture of SiC particle and ethanol, fully stir, mix; C, the said mixture containing SiC nano particle is placed in baking oven toasts, dry, storing temperature is 80 ~ 95 DEG C.
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 745-770 DEG C, 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, stir after all raw materials melt completely, make alloying constituent even, then pretreated nano SiC granule is added, stir again, make it mix,
(3) refining: make smelting furnace be warming up to 785 DEG C ~ 800 DEG C alloys and carry out refining, add heat resistance magnesium alloy refining agent while stirring, refining time is 1-4 minute, 5 ~ 8 minutes are left standstill, consisting of of described heat resistance magnesium alloy refining agent: NaCl:11% ~ 15% 740 DEG C ~ 750 DEG C insulations after refining is complete; Na3AlF6:8 ~ 10%; MgCl2:30-40%; Surplus is KCl;
(4) cast: the magnesium alloy refining material of melting being cast to preheating temperature is in the swage tool of 200 ~ 300 DEG C, and pouring temperature is 730 DEG C ~ 740 DEG C; Cast gauge is Ф 450mm ~ Ф 500mm, length >=3000mm
(5) thermal treatment: foundry goods is carried out solution treatment in 435-440 DEG C of temperature range, the solution treatment time is 16 ~ 24 hours, then carry out shrend, the foundry goods after quenching to be put in the resistance furnace of 210 DEG C artificial aging 40 hours, obtained magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 410 DEG C ~ 450 DEG C 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%, every 3-6 passage forging after annealing 1.5h, and annealing temperature is 410 DEG C ~ 450 DEG C; B. heated roll to temperature is 310-350 DEG C; C. heating slab to temperature is 460-470 DEG C, is incubated after 20-30 minute, and adopt the method for multi-pass small deformation amount that heavy plate rolling is become 2 ~ 10mm thin plate, the speed of rolls is 0.4m/s ~ 0.8 m/s; Every time roll reduction is 10% ~ 20%, melts down annealing after every time rolling, and annealing temperature is 410 DEG C ~ 450 DEG C, and annealing time is 30min ~ 40min;
(7) roll postheat treatment: the thin plate after rolling is carried out ageing treatment, and described aging treatment process is: aging temp is 230-250 DEG C, soaking time is 12-36h; Carry out second time ageing treatment at 200-220 DEG C again, aging time is 12-36h; Finally carry out third time ageing treatment at 150-180 DEG C, aging time is 12-36h.
Further, contain according to weight percent content: 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 the diameter of Mg, SiC nano particle is 50nm.
The invention has the advantages that:
1, on the basis of complex magnesium alloy, by adding nano reinforcement particle, the obdurability of magnesium alloy is improved;
2, develop new nano particle pretreatment technology, make nano particle more effective for adding in the 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 kind of 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 prepares: carry out raw material preparation according to weight percent content, 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, pour appropriate analytical pure ethanol in a reservoir, 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 accounting for said mixture volume 1/40 to be added in the mixture of SiC particle and ethanol, fully stir, mix; C, the said mixture containing SiC nano particle is placed in baking oven toasts, dry, storing temperature is 90 DEG C;
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 750 DEG C, 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, stir after all raw materials melt completely, make alloying constituent even; Then add pretreated nano SiC granule, then stir, make it mix;
(3) refining: make smelting furnace be warming up to 790 DEG C of alloys and carry out refining, add heat resistance magnesium alloy refining agent while stirring, refining time is 4 minutes, leaves standstill 6 minutes, consisting of of described heat resistance magnesium alloy refining agent: NaCl:13% after refining is complete 745 DEG C of insulations; Na3AlF6:9%; MgCl2:35%; Surplus is KCl;
(4) cast: the magnesium alloy refining material of melting being cast to preheating temperature is in the swage tool of 260 DEG C, and pouring temperature is 735 DEG C; Cast gauge is Ф 45, length 3000mm
(5) thermal treatment: foundry goods is carried out solution treatment in 435 DEG C of temperature ranges, the solution treatment time is 24 hours, then carries out shrend, and the foundry goods after quenching to be put in the resistance furnace of 210 DEG C artificial aging 40 hours, obtained magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 410 DEG C of insulation 2h; Carry out two to hammer cogging, be forged into the slab that thickness is 60mm; Reduction in pass is 35%, every 4 passage forging after annealing 1.5h, and annealing temperature is 410 DEG C; B. heated roll to temperature is 350 DEG C; C. heating slab to temperature is 470 DEG C, is incubated after 30 minutes, and adopt the method for multi-pass small deformation amount that heavy plate rolling is become 3mm thin plate, the speed of rolls is 0.7 m/s; Every time roll reduction is 15%, melts down annealing after every time rolling, and annealing temperature is 4100 DEG C, and annealing time is 35min;
(7) roll postheat treatment: the thin plate after rolling is carried out ageing treatment, and described aging treatment process is: aging temp is 245 DEG C, soaking time is 16h; Carry out second time ageing treatment at 215 DEG C again, aging time is 16h; Finally carry out third time ageing treatment at 165 DEG C, aging time is 16h.
embodiment 2:
A kind of 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 prepares: carry out raw material preparation according to weight percent content, 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, pour appropriate analytical pure ethanol in a reservoir, 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 accounting for said mixture volume 1/30 to be added in the mixture of SiC particle and ethanol, fully stir, mix; C, the said mixture containing SiC nano particle is placed in baking oven toasts, dry, storing temperature is 85 DEG C;
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 745-770 DEG C, 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, stir after all raw materials melt completely, make alloying constituent even; Then add pretreated nano SiC granule, then stir, make it mix;
(3) refining: make smelting furnace be warming up to 790 DEG C of alloys and carry out refining, add heat resistance magnesium alloy refining agent while stirring, refining time is 4 minutes, leaves standstill 8 minutes, consisting of of described heat resistance magnesium alloy refining agent: NaCl:13% after refining is complete 740 DEG C of insulations; Na3AlF6:9%; MgCl2:36%; Surplus is KCl;
(4) cast: the magnesium alloy refining material of melting being cast to preheating temperature is in the swage tool of 240 DEG C, and pouring temperature is 38 DEG C; Cast gauge is Ф 480mm, length 3500mm
(5) thermal treatment: foundry goods is carried out solution treatment in 440 DEG C of temperature ranges, the solution treatment time is 16 hours, then carries out shrend, and the foundry goods after quenching to be put in the resistance furnace of 210 DEG C artificial aging 40 hours, obtained magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 435 DEG C of insulation 1.5h; Carry out two to hammer cogging, be forged into the slab that thickness is 45mm; Reduction in pass is 25%, every 3 passage forging after annealing 1.5h, and annealing temperature is 430 DEG C; B. heated roll to temperature is 320 DEG C; C. heating slab to temperature is 465 DEG C, is incubated after 25 minutes, and adopt the method for multi-pass small deformation amount that heavy plate rolling is become 4mm thin plate, the speed of rolls is 0.45 m/s; Every time roll reduction is 12%, melts down annealing after every time rolling, and annealing temperature is 435 DEG C, and annealing time is 35min;
(7) roll postheat treatment: the thin plate after rolling is carried out ageing treatment, and described aging treatment process is: aging temp is 250 DEG C, soaking time is 12h; Carry out second time ageing treatment at 220 DEG C again, aging time is 12h; Finally carry out third time ageing treatment at 180 DEG C, aging time is 12h.
embodiment 3:
A kind of 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 the diameter of Mg, SiC nano particle is 25nm.
The preparation method of described heat resistance magnesium alloy, comprises the following steps:
(1) raw material prepares: carry out raw material preparation according to weight percent content, 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, pour appropriate analytical pure ethanol in a reservoir, 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 accounting for said mixture volume 1/25 to be added in the mixture of SiC particle and ethanol, fully stir, mix; C, the said mixture containing SiC nano particle is placed in baking oven toasts, dry, storing temperature is 92 DEG C;
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 750 DEG C, 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, stir after all raw materials melt completely, make alloying constituent even; Then add pretreated nano SiC granule, then stir, make it mix;
(3) refining: make smelting furnace be warming up to 790 DEG C of alloys and carry out refining, add heat resistance magnesium alloy refining agent while stirring, refining time is 4 minutes, leaves standstill 8 minutes, consisting of of described heat resistance magnesium alloy refining agent: NaCl:13% after refining is complete 740 DEG C of insulations; Na3AlF6:9%; MgCl2:36%; Surplus is KCl;
(4) cast: the magnesium alloy refining material of melting being cast to preheating temperature is in the swage tool of 240 DEG C, and pouring temperature is 38 DEG C; Cast gauge is Ф 480mm, length 3500mm
(5) thermal treatment: foundry goods is carried out solution treatment in 440 DEG C of temperature ranges, the solution treatment time is 16 hours, then carries out shrend, and the foundry goods after quenching to be put in the resistance furnace of 210 DEG C artificial aging 40 hours, obtained magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 435 DEG C of insulation 1.5h; Carry out two to hammer cogging, be forged into the slab that thickness is 45mm; Reduction in pass is 25%, every 3 passage forging after annealing 1.5h, and annealing temperature is 430 DEG C; B. heated roll to temperature is 320 DEG C; C. heating slab to temperature is 465 DEG C, is incubated after 25 minutes, and adopt the method for multi-pass small deformation amount that heavy plate rolling is become 4mm thin plate, the speed of rolls is 0.45 m/s; Every time roll reduction is 12%, melts down annealing after every time rolling, and annealing temperature is 435 DEG C, and annealing time is 35min;
(7) roll postheat treatment: the thin plate after rolling is carried out ageing treatment, and described aging treatment process is: aging temp is 250 DEG C, soaking time is 12h; Carry out second time ageing treatment at 220 DEG C again, aging time is 12h; Finally carry out third time ageing treatment at 180 DEG C, 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: contain according to weight percent content: 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 that the diameter of Mg, 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 prepares: carry out raw material preparation according to weight percent content, 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, pour appropriate analytical pure ethanol in a reservoir, 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 accounting for volume of mixture 1/50 ~ 1/10 to be added in the mixture of SiC particle and ethanol, fully stir, mix; C, the mixture containing SiC nano particle is placed in baking oven toasts, dry, storing temperature is 80 ~ 95 DEG C;
(2) melting: adopt gas atmosphere molten alloy in resistance furnace, smelting temperature is 745-770 DEG C, 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, stir after all raw materials melt completely, make alloying constituent even, then pretreated nano SiC granule is added, stir again, make it mix,
(3) refining: make smelting furnace be warming up to 785 DEG C ~ 800 DEG C alloys and carry out refining, add heat resistance magnesium alloy refining agent while stirring, refining time is 1-4 minute, 5 ~ 8 minutes are left standstill, consisting of of described heat resistance magnesium alloy refining agent: NaCl:11% ~ 15% 740 DEG C ~ 750 DEG C insulations after refining is complete; Na
3alF
6: 8 ~ 10%; MgCl
2: 30-40%; Surplus is KCl;
(4) cast: the magnesium alloy refining material of melting being cast to preheating temperature is in the swage tool of 200 ~ 300 DEG C, and pouring temperature is 730 DEG C ~ 740 DEG C; Cast gauge is Ф 450mm ~ Ф 500mm, length >=3000mm;
(5) thermal treatment: foundry goods is carried out solution treatment in 435-440 DEG C of temperature range, the solution treatment time is 16 ~ 24 hours, then carry out shrend, the foundry goods after quenching to be put in the resistance furnace of 210 DEG C artificial aging 40 hours, obtained magnesium alloy blank;
(6) deformation process: a. high temperature forging cogging: heating blank to temperature is 410 DEG C ~ 450 DEG C 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%, every 3-6 passage forging after annealing 1.5h, and annealing temperature is 410 DEG C ~ 450 DEG C; B. heated roll to temperature is 310-350 DEG C; C. heating slab to temperature is 460-470 DEG C, is incubated after 20-30 minute, and adopt the method for multi-pass small deformation amount that heavy plate rolling is become 2 ~ 10mm thin plate, the speed of rolls is 0.4m/s ~ 0.8 m/s; Every time roll reduction is 10% ~ 20%, melts down annealing after every time rolling, and annealing temperature is 410 DEG C ~ 450 DEG C, and annealing time is 30min ~ 40min;
(7) roll postheat treatment: the thin plate after rolling is carried out ageing treatment, and described aging treatment process is: aging temp is 230-250 DEG C, soaking time is 12-36h; Carry out second time ageing treatment at 200-220 DEG C again, aging time is 12-36h; Finally carry out third time ageing treatment at 150-180 DEG C, aging time is 12-36h.
3. the preparation method of a kind of nano-particle reinforcement multicomponent heat-resistant magnesium alloy as claimed in claim 2, is characterized in that: contain according to weight percent content: 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 the diameter of Mg, SiC nano particle is 50nm.
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| 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 |
| CN104630588B (en) * | 2015-01-04 | 2017-01-04 | 河南科技大学 | A kind of magnesium base composite material and composite pot tool |
| CN104818399A (en) * | 2015-05-12 | 2015-08-05 | 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 thereof |
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| CN105624502B (en) * | 2016-01-15 | 2018-05-04 | 佛山市领卓科技有限公司 | A kind of magnesium alloy of ultra high modulus and preparation method thereof |
| 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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| CN102121074A (en) * | 2011-04-15 | 2011-07-13 | 江苏大学 | Method for preparing nano particle enhanced magnesium-based composite material |
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