CN106834766B - A method of preparing large scale high alloy constituent content magnesium alloy ingot - Google Patents

A method of preparing large scale high alloy constituent content magnesium alloy ingot Download PDF

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CN106834766B
CN106834766B CN201510883275.9A CN201510883275A CN106834766B CN 106834766 B CN106834766 B CN 106834766B CN 201510883275 A CN201510883275 A CN 201510883275A CN 106834766 B CN106834766 B CN 106834766B
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ingot
magnesium
alloy
preheating
melt
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CN106834766A (en
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李永军
张奎
李兴刚
马鸣龙
石国梁
袁家伟
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GRIMN Engineering Technology Research Institute Co Ltd
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

The present invention relates to a kind of methods for preparing large scale high alloy constituent content magnesium alloy ingot, belong to magnesium alloy materials preparation field.The melting that pure magnesium ingot is first carried out in melting furnace is submerged in magnesium melt together with the charging basket for holding them then by the alloying element pure metal ingot or intermediate alloy ingot of preheating, is evenly distributed on all alloying elements in magnesium melt;Magnesium alloy melt is poured into metal casting mould, and it is kept the temperature out of mold upper end downward a certain range using asbestic blanket package mold, it is cooling that slewing is carried out with water since mold bottom simultaneously, then remove mold upper end for heat preservation asbestic blanket, quick water cooling is carried out to asbestic blanket soak zones, demoulds and ingot casting is put into isothermal holding in heat-treatment furnace.Large scale magnesium alloy ingot obtained avoids ingot casting cracking, simultaneously effective eliminates the structural constituent segregation in ingot casting, can be directly used for the deformation processings such as subsequent forging, extruding.

Description

A method of preparing large scale high alloy constituent content magnesium alloy ingot
Technical field
The present invention relates to a kind of methods for preparing large scale high alloy constituent content magnesium alloy ingot, belong to magnesium alloy materials Preparation field.
Background technique
As structural metallic materials most light at present, magnesium alloy has specific strength height, the good, rapid heat dissipation of damping performance etc. very much Advantage makes it all be with a wide range of applications in many fields such as aerospace, automobile, weapons.Not with above-mentioned field Disconnected development, made higher requirement the performance and dimensions of magnesium alloy materials.It is right in actual industrialized production In magnesium alloys such as traditional AZ80, ZK60, in the large scale ingot blank casting process that diameter reaches 600~800mm of Φ, due to casting Inside and outside ingot cooling rate differ greatly, setting time it is long, be easy to produce serious component segregation or that ingot blank center portion cracking occurs be existing As.And for high-strength temperature-resistant but Plastic phase is to relatively low EW75 (Mg-7Gd-5Y-1Nd-0.5Zr), WE83 (Mg-8Y-3Nd- 0.5Zr), the magnesium alloy of the high rare-earth contents such as WE91 (Mg-9Y-1MM-0.5Zr), melting, cast temperature are relatively higher, thermal conductivity Rate is lower, and solidification shrinkage is again very big, and intensity of cooling is small in ingot blank casting process, and setting time is long, and component segregation is serious;It is cooling Intensity is big, and solidification shrinkage is uneven, will generate very big residualinternal stress, easily causes ingot blank center portion cracking, as shown in Figure 1 For the scene of EW75 magnesium alloy large scale ingot casting casting cracking.
Using semi-continuous casting mode, the case where ingotism can be improved, cracked, but for diameter greater than 600mm's The magnesium alloy ingot of magnesium alloy ingot, especially high rare-earth content (being greater than 10wt.%), semi-continuous casting mode are equally difficult to solve The problem of certainly ingot casting internal-external temperature difference in process of setting is big, segregation is serious or even cracks, also generally existing ingot casting surface cold shut is deep, Cause subsequent machining amount big, founding link is at high cost, recovery rate is low.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing large scale high alloy constituent content magnesium alloy ingot, this method Prepared large scale magnesium alloy ingot structural constituent is uniform, residual stress is low, tearing tendency is small, high yield rate, is particularly suitable for The small lot production of the large scale magnesium alloy ingot of high rare-earth content at present.
The method that the present invention prepares large scale high alloy constituent content magnesium alloy ingot, mainly includes the following steps:
(1) using the intermediate alloy ingot of pure magnesium ingot, the pure metal ingot of different-alloy element or they and magnesium as raw material, as needed The weight percent of the magnesium alloy ingredient of preparation is stocked up;
(2) preheating furnace is warming up to 160~660 DEG C, and melting furnace is warming up to 500~800 DEG C, and be passed through to melting furnace Protective gas;
(3) in preheating furnace, pure magnesium ingot is preheating to 100~600 DEG C, while the alloying element pure metal ingot that will need to be added Or in which alloy pig, it is preheating to 100~500 DEG C;
(4) melting that pure magnesium ingot is carried out in the melting furnace having been warmed up, will account for the fusing weight of entire melting furnace first 1/2~1/20 preheating pure magnesium ingot is added in melting furnace, is completely melt it under the protection of protective gas, then by remaining Preheating pure magnesium ingot is added portionwise in melting furnace, after preceding a batch preheating pure magnesium ingot fusing, adds next group preheated magnesium ingot, often Batch additional amount is subject to pure magnesium ingot and is submerged in magnesium melt completely;So repeat, until pure magnesium ingot additional amount reaches predetermined Value, after being completely melt, the dross of molten surface is cleaned out, and temperature is controlled at 680~850 DEG C;
(5) by the alloying element pure metal ingot or in which alloy pig after preheating, together with holding their charging basket It submerges in magnesium melt;
(6) magnesium melt temperature is controlled at 720~850 DEG C, it is complete to alloying element pure metal ingot or in which alloy pig After dissolution, then 720~850 DEG C keep the temperature 10~60 minutes, be evenly distributed on all alloying elements in magnesium melt;
(7) then, magnesium alloy melt is poured into the metal casting mould being fully warmed-up, and from mold upper end to It wraps up mold using asbestic blanket in lower 300~500mm to be kept the temperature, in bell center tapping by armoured thermocouple It is inserted into alloy melt, insertion depth is from the downward 500~600mm in bell position, the temperature change of real-time monitoring alloy melt, together When carry out the cooling 10~60min of slewing with water since mold bottom, when alloy melt temperature is down to 650~700 DEG C, Extract thermocouple, remove mold upper end for heat preservation asbestic blanket, bell is opened, to the quick water cooling of asbestic blanket soak zones progress 1~10min, then quicker de-mold, and be put into have warmed up into 350~500 DEG C of large-scale heat-treatment furnace by ingot casting immediately and keep the temperature 20~60h is air-cooled to room temperature and carries out turnery processing to ingot casting surface after coming out of the stove.
The protective gas is argon gas and CO2Mixed gas, the two volume ratio preferable 3:2.
Preferably, preheating furnace is warming up to 300~350 DEG C, melting furnace is warming up to 600~620 DEG C.
The charging basket is made of mild steel or high chrome, is thick with a large amount of aperture thereon, pure convenient for alloying element The dissolution and diffusion of ingot or in which alloy pig.
The preheating temperature of metal casting mould is 200~500 DEG C;Slewing cooling refers to die surface water cooling height Range:Since bottom, 200mm is ramped up every 2~5min.
Before casting, the step of can also increasing on-the-spot sample analysis;According to being adjusted as a result, determining the need for charging for on-the-spot sample analysis It is whole.Spectrum samples are first poured, on-the-spot sample analysis is carried out, if ingredient and content are unqualified, can feed adjustment, until qualified.
The method of the present invention is suitable for preparation diameter of phi 600mm or more, such as diameter is 600~1000mm of Φ, highly 800~ The magnesium alloy ingot of 1600mm, wherein magnesium alloy can be the magnesium alloy of high alloy constituent content (10wt.% or more), especially The magnesium alloy of high rare-earth content (10wt.% or more).
Using the large scale magnesium alloy ingot of the method for the present invention preparation diameter of phi 600mm or more, casting can not only be eliminated in time The residual stress generated in ingot process of setting, avoids ingot casting from cracking, and simultaneously effective eliminates the structural constituent segregation in ingot casting, It can be directly used for the deformation processings such as subsequent forging, extruding after ingot casting surface machining after Short Time Heating.
Detailed description of the invention
Fig. 1 is the scene of EW75 magnesium alloy large scale ingot casting casting cracking.
Fig. 2-1 and Fig. 2-2 is the appearance and its gold using Φ 650mm EW75 magnesium alloy ingot prepared by the present invention respectively Phase constitution figure.
Fig. 3-1 and Fig. 3-2 is the appearance and its gold using Φ 700mm AZ91 magnesium alloy ingot prepared by the present invention respectively Phase constitution figure.
Specific embodiment
Embodiment 1:The preparation of Φ 600~1000mm EW75 magnesium alloy ingot
1, melting prepares
It stocks up by alloying component proportion, feeds intake and always weigh about 1000Kg.Connect the power supply of preheating furnace, melting furnace, heating. Preheating furnace is warming up to 300~350 DEG C, melting furnace is warming up to 600~620 DEG C, protective gas (argon gas is passed through into melting furnace And CO2Mixed gas, the two volume ratio are about 3:2);
2, pure magnesium ingot preheating and fusing
The 850Kg pure magnesium ingot of clean surface is preheating to 300 DEG C using preheating furnace, guarantees surface without steam.It is firstly added The pure magnesium ingot of 300Kg clean surface is completely melt it under foregoing mixed gas protection, then will be preheating to setting temperature in batches The pure magnesium ingot of degree is added in melting furnace, and specific additional amount is subject to magnesium ingot and is submerged in magnesium liquid completely;Until completely melted again Next group preheated magnesium ingot is added, additional amount is still subject to magnesium ingot and is submerged in magnesium liquid completely;Repeatedly, until magnesium ingot is added Amount reaches predetermined value 850Kg, after being completely melt, stands 5~10min, is cleaned out the dross of molten surface with spoon is skimmed, will Temperature is controlled at 700 DEG C or so;
3, pure Gd, Y, Nd and Mg-30%Zr intermediate alloy ingot preheating
Start to preheat weighted rare earth and Mg-30Zr intermediate alloy (Gd during above-mentioned magnesium liquid is stood:70Kg, Y:50Kg, Nd:10Kg, Mg-30Zr:40Kg), 300~350 DEG C of preheating temperature.Wherein rare earth metal is dispensed into intermediate alloy In two charging baskets, it is put into togerther in preheating furnace and preheats together with charging basket.The basket that feeds is processed using the Cr13 steel plate of 3mm thickness to be made At drilling out the aperture of a large amount of Φ 5mm on the steel plate, be allowed into sieve-like;
4, alloying
Pure rare earth after preheating is submerged in magnesium melt together with the charging basket for holding them, raises simultaneously Serum Magnesium temperature Degree, controls at 820~850 DEG C, 15~20min is kept the temperature after rare earth metal is completely dissolved, and is then added among Mg-30Zr and closes Gold increases electromagnetic frequency until completely dissolved, while carrying out mechanical stirring, makes to be added in 820~850 DEG C of lasting 30min dilute Native alloying element and Zr are evenly distributed in Serum Magnesium;
5, ingot casting is cooling and destressing fire is handled
Above-mentioned magnesium alloy melt is poured into the metal casting mould being fully warmed-up, metal casting mould it is interior Diameter is 600~1000mm, is highly 1000~1600mm, and from the downward 300~400mm in mold upper end, wrapped up using asbestic blanket Mold is kept the temperature, and armoured thermocouple is inserted into alloy melt in bell center tapping, insertion depth is from bell position Downward 500~600mm, the temperature change of real-time monitoring alloy melt are set, while quickly determine with water since mold bottom To cooling (die surface water cooling altitude range:Since bottom, 200mm is ramped up every 2~5min) 20~50min, to When alloy melt temperature is down to 660~680 DEG C, extract thermocouple, remove mold upper end for heat preservation asbestic blanket, opening furnace Lid carries out quick 3~5min of water cooling to asbestic blanket soak zones, then quicker de-mold, and ingot casting is put into immediately have warmed up to 60h is kept the temperature in 500 DEG C of large-scale heat-treatment furnace, room temperature is air-cooled to after coming out of the stove and turnery processing is carried out to ingot casting surface.
Φ 600~1000mm EW75 large scale the magnesium alloy ingot prepared using method of the invention is not only eliminated in time The residual stress generated in Casting Ingot Solidification Process avoids ingot casting cracking, simultaneously effective eliminates being organized into ingot casting Divide segregation, can be directly used for the deformation processings such as subsequent forging, extruding after ingot casting surface machining after Short Time Heating.Such as It is the appearance and metallographic structure using the Φ 650mm EW75 magnesium alloy ingot of this method preparation respectively shown in Fig. 2-1 and Fig. 2-2 Figure, it can be seen that ingot casting smooth in appearance does not crack, and morphological element is uniform.
Embodiment 2:The preparation of Φ 600~1000mm AZ91 magnesium alloy ingot
1, melting prepares
It stocks up by alloying component proportion, feeds intake and always weigh about 1000Kg.Connect the power supply of preheating furnace, melting furnace, heating. Preheating furnace is warming up to 300~350 DEG C, melting furnace is warming up to 600~620 DEG C, protective gas (argon gas is passed through into melting furnace And CO2Mixed gas, the two volume ratio are about 3:2);
2, pure magnesium ingot preheating and fusing
The 900Kg pure magnesium ingot of clean surface is preheating to 300 DEG C using preheating furnace, guarantees surface without steam.It is firstly added The pure magnesium ingot of 300Kg clean surface is completely melt it under foregoing mixed gas protection, then will be preheating to setting temperature in batches The pure magnesium ingot of degree is added in melting furnace, and specific additional amount is subject to magnesium ingot and is submerged in magnesium liquid completely;Until completely melted again Next group preheated magnesium ingot is added, additional amount is still subject to magnesium ingot and is submerged in magnesium liquid completely;Repeatedly, until magnesium ingot is added Amount reaches predetermined value 900Kg, after being completely melt, stands 5~10min, is cleaned out the dross of molten surface with spoon is skimmed, will Temperature is controlled at 700 DEG C or so;
3, pure Al, Zn and Mg-3.0%Mn intermediate alloy ingot preheating
Start to preheat weighted rare earth and Mg-3.0Mn intermediate alloy (Al during above-mentioned magnesium liquid is stood:90Kg, Zn:10Kg, Mg-3.0Mn:20Kg), 300~350 DEG C are preheating to.Wherein pure Al, Zn metal and Mg-3.0Mn intermediate alloy are packed into In one charging basket, it is put into togerther in preheating furnace and preheats together with charging basket.The basket that feeds is processed using the Cr13 steel plate of 3mm thickness to be made At drilling out the aperture of a large amount of Φ 5mm on the steel plate, be allowed into sieve-like;
4, alloying
Pure Al, Zn metal after preheating is submerged into magnesium together with the charging basket for holding them with Mg-3.0Mn intermediate alloy In melt, Serum Magnesium temperature is raised simultaneously, is controlled at 720~750 DEG C, it is complete to pure Al, Zn metal and Mg-3.0Mn intermediate alloy In 720~750 DEG C of 15~20min of heat preservation after fully dissolved, while mechanical stirring is carried out, continuing 30min makes the alloying element being added It is evenly distributed in Serum Magnesium;
5, ingot casting is cooling and destressing fire is handled
Above-mentioned magnesium alloy melt is poured into the metal casting mould being fully warmed-up, metal casting mould it is interior Diameter is 600~1000mm, is highly 1000~1500mm, and about 350mm uses asbestic blanket to wrap up mold downwards from mold upper end Kept the temperature, bell center tapping by armoured thermocouple be inserted into alloy melt in, insertion depth from bell position to Lower about 450mm, the temperature change of real-time monitoring alloy melt, while slewing cooling is carried out with water since mold bottom (die surface water cooling altitude range:Since bottom, 200mm is ramped up every 2~5min) about 20min, to alloy melt When temperature is down to 650 DEG C, extract thermocouple, remove mold upper end for heat preservation asbestic blanket, open bell, to asbestic blanket heat preservation Region carries out quick water cooling about 3min, then quicker de-mold, and ingot casting is put into the large size heat treatment having warmed up to 390 DEG C immediately 40h is kept the temperature in furnace, and room temperature is air-cooled to after coming out of the stove and turnery processing is carried out to ingot casting surface.
Φ 600~1000mm AZ91 large scale the magnesium alloy ingot prepared using method of the invention is not only eliminated in time The residual stress generated in Casting Ingot Solidification Process avoids ingot casting cracking, simultaneously effective eliminates being organized into ingot casting Divide segregation, can be directly used for the deformation processings such as subsequent forging, extruding after ingot casting surface machining after Short Time Heating.Such as It is the appearance and metallographic structure using the Φ 700mm AZ91 magnesium alloy ingot of this method preparation respectively shown in Fig. 3-1 and Fig. 3-2 Figure, it can be seen that ingot casting smooth in appearance does not crack, and morphological element is uniform.

Claims (7)

1. a kind of method for preparing large scale high alloy constituent content magnesium alloy ingot, includes the following steps:
(1) using the intermediate alloy ingot of pure magnesium ingot, the pure metal ingot of different-alloy element or they and magnesium as raw material, according to magnesium alloy The weight percent of ingredient is stocked up;
(2) preheating furnace is warming up to 160~660 DEG C, and melting furnace is warming up to 500~800 DEG C, and be passed through protection to melting furnace Gas;
(3) in preheating furnace, pure magnesium ingot is preheating to 100~600 DEG C, at the same by the alloying element pure metal ingot that need to be added or in Between alloy pig, be preheating to 100~500 DEG C;
(4) melting that pure magnesium ingot is carried out in melting furnace, will account for the preheating of the fusing weight 1/2~1/20 of entire melting furnace first Pure magnesium ingot is added in melting furnace, is completely melt it under the protection of protective gas, then in batches by remaining preheating pure magnesium ingot It is added in melting furnace, after preceding a batch preheating pure magnesium ingot fusing, adds next group preheated magnesium ingot, every batch of additional amount is with pure magnesium Subject to ingot is submerged in completely in magnesium melt;Until pure magnesium ingot additional amount reaches predetermined value, after being completely melt, molten surface is cleared up Dross controls temperature at 680~850 DEG C;
(5) by the alloying element pure metal ingot or intermediate alloy ingot of preheating, it is molten that magnesium is submerged together with the charging basket for holding them In liquid;
(6) magnesium melt temperature is controlled at 720~850 DEG C, after alloying element pure metal ingot or intermediate alloy ingot are completely dissolved, 10~60 minutes are kept the temperature again, are evenly distributed on all alloying elements in magnesium melt;
(7) then, magnesium alloy melt is poured into preheated metal casting mould, the metal casting mould Internal diameter is 600~1000mm, is highly 800~1600mm, and asbestos are used out of mold upper end downward 300~500mm Felt package mold kept the temperature, bell center tapping by armoured thermocouple be inserted into alloy melt in, insertion depth from Downward 500~the 600mm in bell position, the temperature change of real-time monitoring alloy melt, while being carried out since mold bottom with water Slewing cools down 10~60min, when alloy melt temperature is down to 650~700 DEG C, extracts thermocouple, removes mold upper end For the asbestic blanket of heat preservation, bell is opened, quick 1~10min of water cooling is carried out to asbestic blanket soak zones, then quicker de-mold, And ingot casting is put into has warmed up into 350~500 DEG C of heat-treatment furnace 20~60h of heat preservation immediately, room temperature is air-cooled to after coming out of the stove, it is right Ingot casting surface carries out turnery processing.
2. the method for preparation large scale high alloy constituent content magnesium alloy ingot according to claim 1, it is characterised in that: The protective gas is argon gas and CO2Mixed gas.
3. the method for preparation large scale high alloy constituent content magnesium alloy ingot according to claim 2, it is characterised in that: Argon gas and CO2Volume ratio be 3:2.
4. the method for preparation large scale high alloy constituent content magnesium alloy ingot according to claim 1, it is characterised in that: The charging basket is made of mild steel or high chrome, and gather a large amount of aperture thereon.
5. the method for preparation large scale high alloy constituent content magnesium alloy ingot according to claim 1, it is characterised in that: Before casting, increase on-the-spot sample analysis the step of.
6. the method for preparation large scale high alloy constituent content magnesium alloy ingot according to claim 5, it is characterised in that: When on-the-spot sample analysis, if ingredient and content are unqualified, feed adjustment, until qualified.
7. the method for preparation large scale high alloy constituent content magnesium alloy ingot according to claim 1, it is characterised in that: The preheating temperature of the metal casting mould is 200~500 DEG C.
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CN113802038B (en) * 2021-09-03 2022-11-25 中信戴卡股份有限公司 Magnesium alloy for wheel and preparation method thereof
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