CN106834766A - A kind of method for preparing large scale high alloy constituent content magnesium alloy ingot - Google Patents

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

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CN106834766A
CN106834766A CN201510883275.9A CN201510883275A CN106834766A CN 106834766 A CN106834766 A CN 106834766A CN 201510883275 A CN201510883275 A CN 201510883275A CN 106834766 A CN106834766 A CN 106834766A
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ingot
magnesium
alloy
pure
large scale
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CN106834766B (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 method for preparing large scale high alloy constituent content magnesium alloy ingot, belong to magnesium alloy materials preparation field.The melting of pure magnesium ingot is first carried out in melting furnace, the alloying element pure metal ingot or intermediate alloy ingot that then will be preheated are submerged in magnesium melt together with the charging basket for holding them, all alloying elements is evenly distributed in magnesium melt;Magnesium alloy liquation is poured into metal casting mould, and be incubated using asbestic blanket parcel mould from the downward certain limit in mould upper end, simultaneously slewing cooling is carried out since mold bottom with water, then remove mould upper end for be incubated asbestic blanket, asbestic blanket soak zones are carried out with quick water-cooled, ingot casting is simultaneously put into isothermal holding in heat-treatment furnace by the demoulding.Obtained large scale magnesium alloy ingot avoids ingot casting cracking, simultaneously effective eliminates the structural constituent segregation in ingot casting, can be directly used for the deformation processings such as follow-up forging, extruding.

Description

A kind of method for preparing large scale high alloy constituent content magnesium alloy ingot
Technical field
The present invention relates to a kind of method for preparing large scale high alloy constituent content magnesium alloy ingot, belong to magnesium alloy material Material preparation field.
Background technology
Used as structural metallic materials most light at present, magnesium alloy has high, good, rapid heat dissipation of damping performance of specific strength etc. Lot of advantages, makes it be all with a wide range of applications in many fields such as Aero-Space, automobile, weapons.With Above-mentioned field continues to develop, and the performance and dimensions to magnesium alloy materials be proposed requirement higher.In reality In the industrialized production on border, for magnesium alloys such as traditional AZ80, ZK60,600~800mm of Φ are reached in diameter Large scale ingot blank casting process in, due to inside and outside ingot casting cooldown rate differ greatly, setting time it is long, easily produce Serious component segregation or generation ingot blank center portion cracking phenomena.And for high-strength temperature-resistant but Plastic phase to relatively low EW75(Mg-7Gd-5Y-1Nd-0.5Zr)、WE83(Mg-8Y-3Nd-0.5Zr)、WE91 (Mg-9Y-1MM-0.5Zr) magnesium alloy of high rare-earth content such as, its 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, component segregation Seriously;Intensity of cooling is big, and solidification shrinkage is uneven, will produce very big residualinternal stress, easily causes ingot blank Center portion ftractures, and is as shown in Figure 1 the scene of EW75 magnesium alloy large scales ingot casting casting cracking.
Using semi-continuous casting mode, ingotism, the situation of cracking can be improved, but for diameter greater than 600mm Magnesium alloy ingot, the especially magnesium alloy ingot of high rare-earth content (be more than 10wt.%), semi-continuous casting mode Equally it is difficult to solve the problems, such as that ingot casting internal-external temperature difference in process of setting is big, segregation is seriously even ftractureed, also generally deposits In ingot casting surface cold shut depth, cause follow-up machining amount big, founding link high cost, recovery rate are low.
The content of the invention
It is an object of the invention to provide a kind of method for preparing large scale high alloy constituent content magnesium alloy ingot, the party Large scale magnesium alloy ingot structural constituent prepared by method is uniform, residual stress is low, tearing tendency is small, high yield rate, It is particularly suitable for the small lot batch manufacture of the large scale magnesium alloy ingot of current high rare-earth content.
The method that the present invention prepares large scale high alloy constituent content magnesium alloy ingot, mainly comprises the steps:
(1) intermediate alloy ingot with pure magnesium ingot, the pure metal ingot of different-alloy element or they and magnesium is as raw material, The percentage by weight of the magnesium alloy composition for preparing on demand is got the raw materials ready;
(2) preheating furnace is warmed up to 160~660 DEG C, and melting furnace is warmed up to 500~800 DEG C, and to fusing Stove is passed through protective gas;
(3) in preheating furnace, pure magnesium ingot is preheating to 100~600 DEG C, while the alloying element that need to will be added is pure Ingot or its intermediate alloy ingot, are preheating to 100~500 DEG C;
(4) melting of pure magnesium ingot is carried out in the melting furnace having been warmed up, the fusing of whole melting furnace will be accounted for first The preheating pure magnesium ingot of weight 1/2~1/20 is added in melting furnace, it is completely melt under the protection of protective gas, Then remaining preheating pure magnesium ingot is dividedly in some parts in melting furnace, after preceding a collection of preheating pure magnesium ingot melts, then is added Enter next group preheated magnesium ingot, every batch of addition is submerged in magnesium melt and is defined completely by pure magnesium ingot;So repeat, Until pure magnesium ingot addition reaches predetermined value, after being completely melt, the scum silica frost of molten surface is cleaned out, by temperature Control is at 680~850 DEG C;
(5) by the alloying element pure metal ingot or its intermediate alloy ingot after preheating, together with hold they charging basket Submerge together in magnesium melt;
(6) by magnesium melt temperature control at 720~850 DEG C, alloying element pure metal ingot or its intermediate alloy ingot are treated After being completely dissolved, then 10~60 minutes are incubated at 720~850 DEG C, all alloying elements is evenly distributed on magnesium and melt In liquid;
(7) and then, magnesium alloy liquation is poured into the metal casting mould being fully warmed-up, and from mould It is incubated using asbestic blanket parcel mould in the range of the downward 300~500mm in upper end, in the perforate of bell center Place inserts armoured thermocouple in alloy melt, and insertion depth is supervised in real time from the downward 500~600mm in bell position The temperature change of alloy melt is surveyed, while carrying out slewing with water since mold bottom cools down 10~60min, When alloy melt temperature is down to 650~700 DEG C, extract thermocouple, remove mould upper end for be incubated asbestic blanket, Bell is opened, asbestic blanket soak zones is carried out with quick 1~10min of water-cooled, then quicker de-mold, and immediately will casting Ingot is put into and has warmed up into 350~500 DEG C of large-scale heat-treatment furnace 20~60h of insulation, and room temperature is air cooled to after coming out of the stove simultaneously Turnery processing is carried out to ingot casting surface.
Described protective gas is argon gas and CO2Mixed gas, the two volume ratio preferable 3:2.
Preferably, preheating furnace is warmed up to 300~350 DEG C, melting furnace is warmed up to 600~620 DEG C.
Described charging basket is made up of mild steel or high chrome, and substantial amounts of aperture is thick with thereon, is easy to alloying element The dissolving and diffusion of pure metal ingot or its intermediate alloy ingot.
The preheating temperature of metal casting mould is 200~500 DEG C;Slewing cooling refers to that die surface water-cooled is high Degree scope:Since bottom, 200mm is ramped up every 2~5min.
Before cast, the step of can also increase on-the-spot sample analysis;According to the result of on-the-spot sample analysis, it is determined whether need to add Material adjustment.Spectrum samples are first poured into a mould, on-the-spot sample analysis is carried out, if composition and content are unqualified, can feed adjustment, Until qualified.
The inventive method is applied to preparation more than diameter of phi 600mm, such as a diameter of 600~1000mm of Φ, height The magnesium alloy ingot of 800~1600mm, wherein, magnesium alloy can be high alloy constituent content (more than 10wt.%) Magnesium alloy, the especially magnesium alloy of high rare-earth content (more than 10wt.%).
The large scale magnesium alloy ingot of more than diameter of phi 600mm is prepared using the inventive method, can not only be eliminated in time The residual stress produced in Casting Ingot Solidification Process, it is to avoid ingot casting ftractures, and simultaneously effective eliminates the tissue in ingot casting Component segregation, becomes after the machining of ingot casting surface by can be directly used for follow-up forging, extruding etc. after Short Time Heating Shape is processed.
Brief description of the drawings
Fig. 1 is the scene of EW75 magnesium alloy large scales ingot casting casting cracking.
Fig. 2-1 and Fig. 2-2 respectively be using the present invention prepare Φ 650mm EW75 magnesium alloy ingots outward appearance and Its metallographic structure figure.
Fig. 3-1 and Fig. 3-2 respectively be using the present invention prepare Φ 700mm AZ91 magnesium alloy ingots outward appearance and Its metallographic structure figure.
Specific embodiment
Embodiment 1:It is prepared by Φ 600~1000mm EW75 magnesium alloy ingots
1st, melting prepares
Got the raw materials ready by alloying component proportioning, feed intake and always weigh about 1000Kg.Preheating furnace, the power supply of melting furnace are connected, Heat up.Preheating furnace is warmed up to 300~350 DEG C, melting furnace is warmed up to 600~620 DEG C, to being passed through in melting furnace Protective gas (argon gas and CO2Mixed gas, the two volume ratio is about 3:2);
2nd, pure magnesium ingot preheating and fusing
The 850Kg pure magnesium ingots of clean surface are preheating to 300 DEG C using preheating furnace, it is ensured that surface is without steam.First The pure magnesium ingot of 300Kg clean surfaces is added, it is completely melt under foregoing mixed gas protection, then in batches will The pure magnesium ingot for being preheating to design temperature is added in melting furnace, specific addition be submerged in magnesium liquid completely with magnesium ingot in be It is accurate;Add next group preheated magnesium ingot until completely melted, addition be still submerged in magnesium liquid completely with magnesium ingot in be It is accurate;So repeatedly, until magnesium ingot addition reaches predetermined value 850Kg, after being completely melt, 5~10min is stood, With skimming, spoon cleans out the scum silica frost of molten surface, by temperature control at 700 DEG C or so;
3rd, pure Gd, Y, Nd and Mg-30%Zr intermediate alloy ingot preheating
Start preheating weighted rare earth and Mg-30Zr intermediate alloys (Gd during above-mentioned magnesium liquid stands: 70Kg, Y:50Kg, Nd:10Kg, Mg-30Zr:40Kg), 300~350 DEG C of preheating temperature.Its middle rare earth Metal is dispensed into two charging baskets with intermediate alloy, is put into preheating furnace together with charging basket and preheated.Charging basket It is processed into using the thick Cr13 steel plates of 3mm, the aperture of substantial amounts of Φ 5mm is got out on steel plate, is allowed into Sieve-like;
4th, alloying
Pure rare earth after preheating is submerged in magnesium melt together with the charging basket for holding them, while raising Serum Magnesium Temperature, is controlled at 820~850 DEG C, and 15~20min is incubated after rare earth metal is completely dissolved, and is subsequently adding Mg-30Zr Intermediate alloy, increases electromagnetic frequency until completely dissolved, while carrying out mechanical agitation, continues at 820~850 DEG C 30min makes the rare earth alloy element of addition and Zr be evenly distributed in Serum Magnesium;
5th, ingot casting cooling and destressing fire treatment
Above-mentioned magnesium alloy liquation is poured into the metal casting mould being fully warmed-up, metal casting mould Internal diameter is 600~1000mm, is highly 1000~1600mm, and from the downward 300~400mm in mould upper end, It is incubated using asbestic blanket parcel mould, in bell center, armoured thermocouple is inserted alloy melt by tapping In, insertion depth from the downward 500~600mm in bell position, the temperature change of real-time monitoring alloy melt, while Slewing cooling (die surface water-cooled altitude range is carried out with water since mold bottom:Since bottom, often 200mm is ramped up every 2~5min) 20~50min, when alloy melt temperature is down to 660~680 DEG C, pulls out Go out thermocouple, remove mould upper end for be incubated asbestic blanket, opening bell, asbestic blanket soak zones are carried out soon Fast 3~5min of water-cooled, then quicker de-mold, and ingot casting is put into the large-scale heat treatment having warmed up to 500 DEG C immediately 60h is incubated in stove, 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 ingots prepared using the method for the present invention, not only in time Eliminate the residual stress produced in Casting Ingot Solidification Process, it is to avoid ingot casting cracking, simultaneously effective eliminate ingot casting In structural constituent segregation, ingot casting surface machining after by after Short Time Heating i.e. can be directly used for follow-up forging, The deformation processings such as extruding.It is respectively the Φ 650mm EW75 prepared using the method as shown in Fig. 2-1 and Fig. 2-2 The outward appearance and metallographic structure figure of magnesium alloy ingot, it can be seen that ingot casting smooth in appearance, no cracking, and be organized into Part is uniform.
Embodiment 2:It is prepared by Φ 600~1000mm AZ91 magnesium alloy ingots
1st, melting prepares
Got the raw materials ready by alloying component proportioning, feed intake and always weigh about 1000Kg.Preheating furnace, the power supply of melting furnace are connected, Heat up.Preheating furnace is warmed up to 300~350 DEG C, melting furnace is warmed up to 600~620 DEG C, to being passed through in melting furnace Protective gas (argon gas and CO2Mixed gas, the two volume ratio is about 3:2);
2nd, pure magnesium ingot preheating and fusing
The 900Kg pure magnesium ingots of clean surface are preheating to 300 DEG C using preheating furnace, it is ensured that surface is without steam.First The pure magnesium ingot of 300Kg clean surfaces is added, it is completely melt under foregoing mixed gas protection, then in batches will The pure magnesium ingot for being preheating to design temperature is added in melting furnace, specific addition be submerged in magnesium liquid completely with magnesium ingot in be It is accurate;Add next group preheated magnesium ingot until completely melted, addition be still submerged in magnesium liquid completely with magnesium ingot in be It is accurate;So repeatedly, until magnesium ingot addition reaches predetermined value 900Kg, after being completely melt, 5~10min is stood, With skimming, spoon cleans out the scum silica frost of molten surface, by temperature control at 700 DEG C or so;
3rd, pure Al, Zn and Mg-3.0%Mn intermediate alloy ingot preheating
Start preheating weighted rare earth and Mg-3.0Mn intermediate alloys (Al during above-mentioned magnesium liquid stands: 90Kg, Zn:10Kg, Mg-3.0Mn:20Kg), 300~350 DEG C are preheating to.Wherein pure Al, Zn metal Load in a charging basket with Mg-3.0Mn intermediate alloys, be put into preheating furnace together with charging basket and preheated.Plus Charging basket is processed into using the thick Cr13 steel plates of 3mm, and the aperture of substantial amounts of Φ 5mm is got out on steel plate, is made Into sieve-like;
4th, alloying
Pure Al, Zn metal and Mg-3.0Mn intermediate alloys after by preheating do not have together with the charging basket for holding them Enter in magnesium melt, while raising Serum Magnesium temperature, control at 720~750 DEG C, treat pure Al, Zn metal and Mg-3.0Mn Intermediate alloy is incubated 15~20min after being completely dissolved at 720~750 DEG C, while carrying out mechanical agitation, continues 30min The alloying element of addition is set to be evenly distributed in Serum Magnesium;
5th, ingot casting cooling and destressing fire treatment
Above-mentioned magnesium alloy liquation is poured into the metal casting mould being fully warmed-up, metal casting mould Internal diameter is 600~1000mm, is highly 1000~1500mm, and about 350mm is used downwards from mould upper end Asbestic blanket parcel mould is incubated, in armoured thermocouple is inserted alloy melt by bell center tapping, Insertion depth is from bell position about 450mm, the temperature change of real-time monitoring alloy melt, while from mould bottom downwards Portion starts to carry out slewing cooling (die surface water-cooled altitude range with water:Since bottom, every 2~5min Ramp up 200mm) about 20min, when alloy melt temperature is down to 650 DEG C, thermocouple is extracted, remove mould Tool upper end is used for the asbestic blanket being incubated, and opens bell, asbestic blanket soak zones is carried out with quick water-cooled about 3min, so Quicker de-mold afterwards, and be put into have warmed up by ingot casting immediately and be incubated 40h into 390 DEG C of large-scale heat-treatment furnace, come out of the stove After be air cooled to room temperature and turnery processing carried out to ingot casting surface.
Φ 600~1000mm AZ91 large scale the magnesium alloy ingots prepared using the method for the present invention, not only in time Eliminate the residual stress produced in Casting Ingot Solidification Process, it is to avoid ingot casting cracking, simultaneously effective eliminate ingot casting In structural constituent segregation, ingot casting surface machining after by after Short Time Heating i.e. can be directly used for follow-up forging, The deformation processings such as extruding.It is respectively the Φ 700mm AZ91 prepared using the method as shown in Fig. 3-1 and Fig. 3-2 The outward appearance and metallographic structure figure of magnesium alloy ingot, it can be seen that ingot casting smooth in appearance, no cracking, and be organized into Part is uniform.

Claims (8)

1. a kind of method for preparing large scale high alloy constituent content magnesium alloy ingot, comprises the following steps:
(1) intermediate alloy ingot with pure magnesium ingot, the pure metal ingot of different-alloy element or they and magnesium is as raw material, Percentage by weight according to magnesium alloy composition is got the raw materials ready;
(2) preheating furnace is warmed up to 160~660 DEG C, and melting furnace is warmed up to 500~800 DEG C, and to fusing Stove is passed through protective gas;
(3) in preheating furnace, pure magnesium ingot is preheating to 100~600 DEG C, while the alloying element that need to will be added is pure Ingot or intermediate alloy ingot, are preheating to 100~500 DEG C;
(4) melting of pure magnesium ingot is carried out in melting furnace, the fusing weight 1/2~1/20 of whole melting furnace will be accounted for first Preheating pure magnesium ingot add melting furnace in, it is completely melt under the protection of protective gas, it is then that remaining is pre- Hot pure magnesium ingot is dividedly in some parts in melting furnace, after after preceding a collection of preheating pure magnesium ingot fusing, adds next group preheating magnesium Ingot, every batch of addition is submerged in magnesium melt and is defined completely by pure magnesium ingot;Until pure magnesium ingot addition reaches predetermined value, After being completely melt, the scum silica frost of molten surface is cleared up, by temperature control at 680~850 DEG C;
(5) will preheat alloying element pure metal ingot or intermediate alloy ingot, together with hold they charging basket Submerge in magnesium melt;
(6) by magnesium melt temperature control at 720~850 DEG C, treat that alloying element pure metal ingot or intermediate alloy ingot are complete After CL, then 10~60 minutes are incubated, all alloying elements is evenly distributed in magnesium melt;
(7) and then, magnesium alloy liquation is poured into preheated metal casting mould, and from mould upper end It is incubated using asbestic blanket parcel mould in the range of downward 300~500mm, in bell center, tapping will In armoured thermocouple insertion alloy melt, insertion depth is closed from the downward 500~600mm in bell position, real-time monitoring The temperature change of golden melt, while carrying out slewing with water since mold bottom cools down 10~60min, waits to close When golden melt temperature is down to 650~700 DEG C, extract thermocouple, remove mould upper end for be incubated asbestic blanket, beat Asbestic blanket soak zones are carried out quick 1~10min of water-cooled, then quicker de-mold by blow-on lid, and immediately by ingot casting It is put into and has warmed up into 350~500 DEG C of heat-treatment furnace 20~60h of insulation, room temperature is air cooled to after coming out of the stove, to ingot casting Surface carries out turnery processing.
2. the method for preparing large scale high alloy constituent content magnesium alloy ingot according to claim 1, it is special Levy and be:Described protective gas is argon gas and CO2Mixed gas.
3. the method for preparing large scale high alloy constituent content magnesium alloy ingot according to claim 2, it is special Levy and be:Argon gas and CO2Volume ratio be 3:2.
4. the method for preparing large scale high alloy constituent content magnesium alloy ingot according to claim 1, it is special Levy and be:Described charging basket is made up of mild steel or high chrome, and gather substantial amounts of aperture thereon.
5. the method for preparing large scale high alloy constituent content magnesium alloy ingot according to claim 1, it is special Levy and be:Before cast, increase on-the-spot sample analysis the step of.
6. the method for preparing large scale high alloy constituent content magnesium alloy ingot according to claim 5, it is special Levy and be:During on-the-spot sample analysis, if composition and content are unqualified, charging adjustment, until qualified.
7. the method for preparing large scale high alloy constituent content magnesium alloy ingot according to claim 1, it is special Levy and be:The preheating temperature of described metal casting mould is 200~500 DEG C.
8. the method for preparing large scale high alloy constituent content magnesium alloy ingot according to claim 1, it is special Levy and be:The internal diameter of described metal casting mould is 600~1000mm, is highly 800~1600mm.
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