CN104651693B - Microscale Al-containing rare earth wrought magnesium alloy and preparation method thereof - Google Patents

Microscale Al-containing rare earth wrought magnesium alloy and preparation method thereof Download PDF

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Publication number
CN104651693B
CN104651693B CN201310597670.1A CN201310597670A CN104651693B CN 104651693 B CN104651693 B CN 104651693B CN 201310597670 A CN201310597670 A CN 201310597670A CN 104651693 B CN104651693 B CN 104651693B
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temperature
alloy
rare earth
melt
furnace
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CN104651693A (en
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马鸣龙
张奎
李兴刚
李永军
袁家伟
石国梁
张国栋
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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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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/06Alloys based on magnesium with a rare earth metal as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

Abstract

The invention relates to a microscale Al-containing rare earth wrought magnesium alloy and its preparation method and belongs to the scope of industrial magnesium alloy. The magnesium alloy comprises, by weight, 6.5-15.0% of Gd, 3.0-5.5% of Y, 2.0-4.0% of Zn, 0.3-1.5% of Nd, 0.3-0.9% of Zr, 0.4-1.0% of Al and the balance of Mg. The preparation method of the magnesium alloy comprises the steps as follows: raw material preparation, alloy melting, alloy semi-solid extrusion, homogenization treatment, redeformation, cooling and pre-stretching treatment, ageing strengthening treatment and the like. By fully utilizing the defect that Al is preferentially combined with rare earth and Zr in alloy to form a stable phase, Zn element is added to make up insufficiencies and the wrought magnesium alloy with high performance is prepared. The recovery effect of rare earth elements is enhanced, and semi-solid forming and solid plastic forming are combined.

Description

Rare earth wrought magnesium alloy containing trace of Al and preparation method thereof
Technical field
The present invention relates to a kind of rare earth wrought magnesium alloy containing minor-alloying element Al and preparation method thereof, belong to industrial magnesium and close The category of gold.
Background technology
Magnesium-rare earth is the magnesium alloy materials of the relatively broad class of research, and wherein Mg-Gd-Y-Zr alloys are used as a class Typical magnesium-rare earth is one of focus of current research.Because the solid solubility of Gd, Y element in magnesium is larger, dropped with temperature Low solid solubility is reduced rapidly, can carry out ageing strengthening, therefore Mg-Gd-Y-Zr alloys are the heat-treatable strengthened alloys of a class. Cast magnesium alloy has preferable forming property due to it, therefore is widely deployed application, but common in addition to Special Processes of Metal Castings alloy There is casting flaw in casting magnesium alloy, limit its application as load-carrying member high unavoidably, and wrought magnesium alloy has Outstanding and stabilization mechanical property, is the inexorable trend of magnesium alloy development.At present, it is domestic not prepare large-scale deformed Mg conjunction specially The equipment of gold, often relies on existing aluminium alloy former to be prepared processing, such as extrude, roll and forge etc., can cause Contain minor-alloying element Al in alloy, influence the degree of purity of magnesium alloy, the final performance for deteriorating alloy.
Mainly it is that Al is easy to and Zr and Mn in general, Al is not added in the magnesium alloy containing Zr and containing Mn Reaction generation harmful phase, not only reduces the effect of original Zr and Mn, the deteriorate drastically alloy of meeting of simultaneous reactions generation Tissue, is unfavorable for the following process and military service performance of material, and the magnesium-rare earth of crystal grain thinning is carried out in particular with Zr.In addition, In magnesium-rare earth, after being mixed into a certain amount of Al, in addition to the presence of Al-Zr phases, Al can also be with RE reaction generations Al-RE Phase, lowers rare earth solid solution aging invigoration effect in the magnesium alloy, particularly to the rare earth element of solid solubility high, therefore, tradition On the strict presence for preventing Al in Mg-RE-Zr alloy systems.
Al elements that magnesium-rare earth is mixed into clout after plastic working can only be done and be degraded so that it can not reclaimed It is a small amount of to utilize, or directly carry out harmless treatment.But, rare earth is non-renewable resources, it is clear that above-mentioned processing method can be caused The waste of a large amount of rare earths, improves the preparation cost of magnesium alloy, and environment is polluted.Research finds that Al-RE phases have Good heat endurance, can produce during solidification, and phase in version does not occur in the solid state, and the characteristic is in AZ series alloys In be widely applied, but in magnesium-rare earth, typically as unfavorable factor, avoid as far as possible.Ground according to above-mentioned Study carefully result, using Al-RE phases the characteristics of high temperature has heat endurance, develop the alloy that a class can be on active service at high temperature, have There is particularly significant meaning, especially for the recovery that clout is processed due to incidentally adding the rare earth alloy of aluminium in process, can The cost of alloy exploitation is greatly lowered.Research in addition shows that Zn elements are added in rare earth alloy, can form Icosahedral phases or length Cycle ordered structure, can increase substantially the plasticity of alloy after deformation, therefore, Zn elements can be suitably supplemented in the middle of the present invention, use To eliminate the adverse effect that the alloy plasticity caused by the addition of Al elements declines.
The content of the invention
The main object of the present invention is to solve to process clout time due to the magnesium-rare earth for incidentally adding aluminium in process The problem of receipts, by designing the composition of this alloy and the technique of preparation method, under the premise of acquisition is high performance, reduces rare earth magnesium The preparation cost of alloy.
To realize above-mentioned target, the present invention is adopted the following technical scheme that:
A kind of rare earth wrought magnesium alloy containing minor-alloying element Al, its percentage by weight constitutes and is:Gd:6.5~15.0%, Y: 3.0~5.5%, Zn:2.0~4.0%, Nd:0.3~1.5%, Zr:0.3~0.9%, Al:0.4~1.0%, balance of Mg.
There is it to act on per dvielement in body series alloy, rare earth element(Including Gd, Y, Nd)It is main in the formation of alloy Hardening constituent, the characteristics of there is certain solid solubility using it, can be with ageing strengthening alloy;Zn elements are mainly and rare earth element shape Growth cycle ordered structure(LPSO phases), the presence of the phase can largely improve the moulding of alloy;Zr elements can be thin The crystallite dimension of alloy;Al elements can form Al-RE phases with rare earth element, improve the resistance to elevated temperatures of alloy.
A kind of preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al, comprises the following steps:
(1)Raw material prepares, and mode has following two:
Design object alloy of the invention is:
Mg- (6.5~15.0) Gd- (3.0~5.5) Y- (2.0-4.0) Zn- (0.3~1.5) Nd- (0.3~0.9) Zr- (0.4-1.0)Al
Got the raw materials ready by the percentage by weight of design magnesium alloy composition of the invention;Or closed using the rare earth magnesium after deformation Golden discard, by composition test, adds Al and/or Zn;
(2)Alloy melting
Preheating furnace is warmed up to 300 DEG C~400 DEG C, and melting furnace is warmed up to 600 DEG C~900 DEG C, while to above-mentioned two Protective gas is passed through in individual stove;After raw material is preheated in the preheating furnace respectively, being added in the smelting furnace of preheating carries out alloy and melts Refining, to after being completely melt, adds ultrasonic device and agitating device, and mechanical agitation and ultrasonically treated is carried out to liquation;
(3)Alloy semi-solid is extruded
After stirring, mechanical agitation and ultrasonic processing apparatus are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, 600 DEG C~650 DEG C are cooled to, 10min is incubated, semi-solid state extrusion are carried out, between a diameter of 10mm~200mm of extruded barses;
(4)Cooling and pre-stretching treatment
Alloy after deformation is cooled down in 80 DEG C~150 DEG C recyclable hardening medias, when bar temperature is situated between with quenching Taken out when matter temperature is consistent;The bar for shaping carries out pre-stretching treatment, eliminates residual stress and orthopedic, pre-tension deformation amount It is 2~5%;
(5)Ageing strengthening is processed
Bar with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature 150 DEG C~ Between 250 DEG C, the time be 8h~100h between, subsequent air cooling.
The above method is applied to the processing of the material of semi-solid state extrusion diameter of rod≤50mm, and direct aging is simultaneously cooled down, i.e., Perform step(4)With(5), remaining size material extruding after be directly placed into homogenization heat-treatment furnace in carry out Homogenization Treatments.
The bar of 50mm~100mm a diameter of for semi-solid state extrusion, in step(3)Afterwards, it is further comprising the steps of:
(3)-A Homogenization Treatments
By the control of bar tapping temperature at 500 DEG C ± 10 DEG C, it is then placed in the homogenization heat-treatment furnace for having heated up in advance, Between 500 DEG C~540 DEG C, soaking time is in 8h~48h for homogenization temperature;
(3)-B1 redeformations
Carry out secondary extrusion, extrusion temperature is homogenization temperature, extrusion speed is 5mm~15mm/min, extrusion speed with Extrusion ratio is in inverse ratio, and extrusion ratio controlled quentity controlled variable is 4~25.
Bar for semi-solid state extrusion with diameter greater than 100mm, in step(3)Afterwards, it is further comprising the steps of:
(3)-A Homogenization Treatments
By the control of bar tapping temperature at 500 DEG C ± 10 DEG C, it is then placed in the homogenization heat-treatment furnace for having heated up in advance, Between 500 DEG C~540 DEG C, soaking time is in 8h~48h for homogenization temperature;
(3)-B2 redeformations
2~5 multiway forgings are carried out after homogenization, is not lowered the temperature in deformation process, maintain the temperature at 500 DEG C~550 DEG C, often Insulation 30min~100min is melted down after secondary forging, is then extruded, rolled or direct forging and molding.
Step(1)In, Zr is added in Mg-Zr intermediate alloys form, and in described Mg-Zr intermediate alloys, the composition of Zr contains It is 30~40wt% to measure, and remaining is Mg;Other alloying elements, including remaining Mg and Zn, Al, Gd, Y and Nd are with simple metal Form is added.
Raw material is reclaimed using clout, and the magnesium-rare earth discard car after deformation is fallen into crust, reduces impurity.In fusion process Middle on-line checking Al content, during if fewer than 0.4%, is then supplemented according to volume mass.
In the present invention, according to RE(Rare earth metal)Recovery rate is 85%, Zr recovery rates for 25%, Al recovery rates are 100%, Zn Recovery rate is 90%, calculates the addition weight of alloying element.
Step(2)In, preheating furnace is resistance furnace, and melting furnace is the intermediate frequency electromagnetic induction heater of controllable temperature;Protective gas It is argon gas and 134a mixed gas, the two volume ratio is about 20:1, similarly hereinafter.
New alloy melting comprises the following steps:
Alloy melting is carried out in the smelting furnace having been warmed up:To account for first gross weight 50% it is preheated after pure magnesium ingot Be put into smelting furnace, remaining magnesium ingot added after being completely melt, period temperature control at 660 DEG C~720 DEG C, keep 5min~ 10min, stirs and excludes scum silica frost;The slow rare earth metal for raising melt temperature, adding preheating, adds after magnesium ingot is completely melt When ensure melt temperature be not less than 750 DEG C;It is slow after melt middle rare earth metal dissolves completely to raise melt temperature, add pre- The Mg-Zr intermediate alloys of heat, ensure melt temperature between 800 DEG C~850 DEG C during addition;The Al of preheating is added, during addition More than 800 DEG C, Al particle diameters are 1 centimetre of size to melt temperature, are sufficiently stirred for melt, and 30min is incubated at 800 DEG C, are then lowered the temperature To 750 DEG C;Zn is added, is sufficiently stirred for, now ensure that fluid temperature is not less than 750 DEG C.After being completely melt, add ultrasonic device with And agitating device, mechanical agitation and ultrasonically treated is carried out to liquation.
In preheating furnace, pure magnesium ingot is preheating to 350 DEG C~400 DEG C, continues more than 5min (generally 10min- 20min), it is ensured that magnesium ingot surface is without steam;Rare earth metal, Al and Mg-Zr intermediate alloys are preheating to same temperature in addition, in advance Heated succession is respectively:Rare earth element → Al → Mg-Zr intermediate alloys, more than preheating time 10min, it is ensured that surface is without steam.
Clout reclaims melting and comprises the following steps:
1)Meet Mg- (6.5~15.0) Gd- (3.0~5.5) Y- (0.3~1.5) Nd- (0.3~0.9) after by deformation The magnesium-rare earth clout cutting of Zr compositions is blocking, and volume ratio is close to 3:3:4, preheated together under a shielding gas, the time In 20min~40min;
2)One fritter clout is put into crucible, 600 DEG C~800 DEG C are warming up to, 20min~40min is incubated after fusing, so Skimming afterwards;It is put into second block of fritter clout so that clout is completely melt that insulation 20min~40min removes surface scum;It is put into 3rd block of bulk clout, until completely melted, is incubated 20min~40min, is sufficiently stirred for, skimming operation;
3)On-line period, carries out composition test, and Al is added when Al constituent contents are less than 0.4%, if meeting composition needs, Subsequent step is then carried out, 750 DEG C are then cooled to;
4)Zn is added, is sufficiently stirred for, now ensure that fluid temperature is not less than 750 DEG C.
After being completely melt, ultrasonic device and agitating device are added, mechanical agitation and ultrasonically treated is carried out to liquation.
Described mechanical agitation rotating speed is 60~150rad/min, and ultrasonic power is 3kW~10kW, and melt temperature is maintained at Between 750 DEG C -800 DEG C, action time is 20min-50min, makes mechanical agitation and ultrasonically treated while acting on melt.
Step(3)In, in 5mm-20mm/s, diameter is proportional with extruding for extruder outlet speed.
In step (3)-B2, do not melted down after the extruding or roll forming after multiway forging, the conjunction shaped using multiway forging Do not melted down after golden last time multiway forging.
Step(4)In, described hardening media includes coolant and quenching oil.
Advantages of the present invention:
Take full advantage of Al preferentially with alloy in rare earth and Zr formed stable phase shortcoming, auxiliary with the addition of Zn unit usually Compensate its defect, be prepared for being improve with high performance wrought magnesium alloy the recovering effect of rare earth element, while by semisolid Shaping is combined with solid plastics shaping, is an important innovative point of the invention.
Brief description of the drawings
Fig. 1-1 and Fig. 1-2 is that physical field of the invention stirs schematic diagram, wherein, Fig. 1-1 is ultrasonic device and stirring dress Put, Fig. 1-2 is top view.
Fig. 2-1 and Fig. 2-2 is multiway forging schematic diagram(A time).
Main Reference Numerals:
The ultrasound electric machine of 1 stirring motor 2
The mechanical agitation bar of 3 ultrasonic horn 4
The device pad of 5 impeller 6
Specific embodiment
The preparation method of rare earth wrought magnesium alloy of the present invention containing minor-alloying element Al, comprises the following steps:
1 material prepares.
Material stand-by mode has following two:
(1) new alloy
Got the raw materials ready by the percentage by weight of design magnesium alloy composition of the invention;Wherein, Zr is with Mg-Zr intermediate alloys Got the raw materials ready, in the intermediate alloy, the component content of Zr is 30~40wt%, and remaining is Mg;In removing intermediate alloy Mg-Zr Mg, the Mg in remaining magnesium alloy is got the raw materials ready with pure magnesium ingot;Gd, Y, Nd are added with form of pure metal.
(2) clout is reclaimed
Magnesium-rare earth discard car after deformation is fallen into crust, impurity is reduced.The on-line checking Al content in fusion process, During if fewer than 0.4%, then supplemented according to volume mass.
2-in-1 golden melting
(1) preheating furnace is warmed up to 300 DEG C~400 DEG C, and melting furnace is warmed up into 600 DEG C~900 DEG C, and (preheating furnace is electricity Resistance stove, melting furnace is the intermediate frequency electromagnetic induction heater of controllable temperature), while (being to protective gas is passed through in above-mentioned two stove Argon gas and 134a mixed gas, the two volume ratio are about 20:1, similarly hereinafter);
1) new alloy melting.
A) in preheating furnace, pure magnesium ingot is preheating to 350 DEG C~400 DEG C, continues more than 5min (generally 10min- 20min), it is ensured that magnesium ingot surface is without steam;Rare earth metal, Al and Mg-Zr intermediate alloys are preheating to same temperature in addition, in advance Heated succession is respectively:Rare earth element → Al → Mg-Zr intermediate alloys, more than preheating time 10min, it is ensured that surface is without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.To account for first total amount 50% it is preheated after pure magnesium ingot It is put into smelting furnace, it is completely melt under the protection of protective gas, be subsequently adding remaining magnesium ingot, whole process is by temperature control System keeps 5min-10min at 660 DEG C -720 DEG C under this state, stirs and exclude scum silica frost.
C) rare earth metal is added, when adding magnesium ingot to be completely melt slow rising melt temperature simultaneously, the dilute of advance preheating is added Earth metal, ensures that the temperature of melt is not less than 750 DEG C during addition;
D) Mg-Zr intermediate alloys are added, it is slow after melt middle rare earth dissolves completely to raise melt temperature, add pre- in advance The Mg-Zr intermediate alloys of heat, ensure melt temperature between 800 DEG C -850 DEG C during addition.
E) Al of the preheating in composition range is added, more than 800 DEG C, particle diameter is 1 centimetre of size to melt temperature during addition. After addition, melt is sufficiently stirred for, 30min is incubated at 800 DEG C, be then cooled to 750 DEG C.
2) clout is reclaimed
A) by deformation after meet Mg- (6.5~15.0) Gd- (3.0~5.5) Y- (0.3~1.5) Nd- (0.3~0.9) The magnesium-rare earth of Zr compositions carries out composition test, if Al constituent contents be less than 0.4%, will in fusion process according to The weight auxiliary addition of 100% recovery rate.
B) clout is cut blocking, it is ensured that size is close to 3:3:4 (volume ratios), are preheated together under a shielding gas, Time is in 20min-40min.
C) fritter clout is put into crucible, is warming up to 600 DEG C -800 DEG C, 20min-40min is incubated after fusing, then skimmed Slag;It is put into second block of fritter clout so that clout is completely melt that insulation 20min-40min removes surface scum;It is put into the 3rd Block bulk clout, until completely melted, is incubated 20min-40min, is sufficiently stirred for, skimming operation.
D) on-line period, carries out composition test, and Al is then added during less than default content, if meeting composition needs, carries out Subsequent step, is then cooled to 750 DEG C.
(2) addition of Zn
Zn is received and must be added in above two melt according to 90%, is sufficiently stirred for, now ensure that fluid temperature is not less than 750℃。
(3) physical field stirring
Be slowly added to ultrasonic device and agitating device, its schematic diagram as shown in Fig. 1-1 and Fig. 1-2, allow mechanical agitation and It is ultrasonically treated while acting on melt (mechanical agitation rotating speed 60-150rad/min, ultrasonic power 3kW-10kW).Now melt temperature Degree is maintained between 750 DEG C -800 DEG C, and action time is in 20min-50min.
Physical field agitating device of the invention includes stirring motor 1, ultrasound electric machine 2, ultrasonic horn 3, mechanical agitation bar 4, leaf Wheel 5 and device pad 6.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation poured into the chamber of semi-solid state extrusion machine, be cooled to 600 DEG C- 650 DEG C, 10min is incubated, carries out semi-solid state extrusion, the diameter of extruded barses is general between 10mm-200mm, extruder outlet Speed is proportional with diameter in 5mm-20mm/s.The material direct aging of diameter≤50mm is simultaneously cooled down(Perform 6 and 7), remaining chi Very little material carries out Homogenization Treatments during homogenization heat-treatment furnace is directly placed into after extruding.
4 Homogenization Treatments
Material tapping temperature with diameter greater than 50mm is controlled at 500 DEG C ± 10 DEG C, and be then placed in having heated up in advance is uniform Change in heat-treatment furnace, between 500 DEG C -540 DEG C, soaking time is in 8h-48h for homogenization temperature.
5 redeformations
(1) diameter directly carries out secondary extrusion in the bar of 50mm-100mm, and extrusion temperature is homogenization temperature, extruding speed It is 5mm-15mm/min to spend, and extrusion speed is in inverse ratio with extrusion ratio, and extrusion ratio controlled quentity controlled variable is in 4-25.
(2) material with diameter greater than 100mm, directly carries out multiway forging 2-5 times, such as Fig. 2-1 and 2-2 institutes after homogenization Show.Do not lower the temperature in deformation process, maintain the temperature at 500 DEG C -550 DEG C, between every time forging after melt down insulation 30min- 100min, is then extruded, is rolled or direct forging and molding.Do not melted down after extruding or roll forming after multiway forging, profit Do not melted down after alloy last time multiway forging with multiway forging shaping.
6 coolings and pre-stretching treatment
By directly cooling (including coolant or the quenching in 80 DEG C of recyclable -150 DEG C of hardening medias of the alloy after deformation Oil), taken out when material temperature is consistent with hardening media temperature;The bar for finally shaping needs to carry out pre-stretching treatment, Elimination residual stress is simultaneously orthopedic, and pre-tension deformation amount is 2-5%.
7 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature 150 DEG C- Between 250 DEG C, the time is between 8h-100h.To after the time, air cooling is taken out.
Present disclosure is described in detail with specific embodiment below.
Embodiment 1
This example molten alloy composition is Mg-6.5Gd-3.0Y-2.0Zn-0.3Nd-0.3Zr-0.4Al.(RE recovery rates are 85%, Zr recovery rate are that 25%, Al recovery rates are that 100%, Zn recovery rates are 90%)
1 material prepares
Zr is got the raw materials ready with Mg-Zr intermediate alloys, and in the intermediate alloy, the component content of Zr is 30%, and remaining is Mg;The Mg in intermediate alloy Mg-Zr is removed, the Mg in remaining magnesium alloy is got the raw materials ready with pure magnesium ingot;Gd, Y, Nd are with proof gold Category form is added, and design addition is:
The alloy of table 1 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 2.It is to ensure rapid melting, raw material is cut into small pieces, size is being smoothly put into Crucible is defined, and removes surface and oil contaminant, and sand papering removes oxide layer.
The actual raw material addition of the 2-in-1 gold of table
2-in-1 golden melting
(1) preheating furnace is warmed up to 300 DEG C, and melting furnace is warmed up into 600 DEG C, and (preheating furnace is resistance furnace, and melting furnace is The intermediate frequency electromagnetic induction heater of controllable temperature), while (being that argon gas and 134a mix to protective gas is passed through in above-mentioned two stove Gas, the two volume ratio is about 20:1, similarly hereinafter);
A) in preheating furnace, pure magnesium ingot is preheating to 300 DEG C, continues 10min, it is ensured that magnesium ingot surface is without steam;In addition will Rare earth metal, Al, Zn and Mg-Zr intermediate alloy are preheating to same temperature, and pre- heated succession is respectively:Rare earth element → Al → Zn → Mg-Zr intermediate alloys, preheating time 10min, it is ensured that surface is without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.To account for first total amount 50% it is preheated after pure magnesium ingot It is put into smelting furnace, it is completely melt under the protection of protective gas, be subsequently adding remaining magnesium ingot, whole process is by temperature control System keeps 5min at 660 DEG C under this state, stirs and exclude scum silica frost.
C) add rare earth metal, when plus magnesium ingot be completely melt it is simultaneously slow raise melt temperature, add in advance the Gd of preheating, Y pure rare earths, ensure 800 DEG C of the temperature of melt during addition;It is slow after melt middle rare earth dissolves completely to raise melt temperature, add The Mg-Zr intermediate alloys of preheating, ensure that melt temperature is 850 DEG C in advance during addition.
D) Al of the preheating in composition range is added, at 800 DEG C, particle diameter is 1 centimetre of size to melt temperature during addition.Add Afterwards, melt is sufficiently stirred for, the Zn that then will be preheated is added in melt, is sufficiently stirred for, and 30min is incubated at 800 DEG C, is then cooled to 750℃。
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 60rad/min, ultrasonic power 3kW).Now melt temperature is maintained at 800 DEG C.Action time is in 20min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 600 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 10mm of extruded barses, extruder outlet speed 5mm/s.
4 coolings and pre-stretching treatment
Alloy after deformation is directly cooled down in 80 DEG C of recyclable coolants, when material temperature and hardening media temperature Taken out when consistent, carry out pre-stretching treatment, elimination residual stress is simultaneously orthopedic, and pre-tension deformation amount is 2%.
5 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 180 DEG C, when Between be 50h.To after the time, air cooling is taken out.
The alloy that deformation is obtained has applied at elevated temperature performance very high, stabilization can be used at 250 DEG C, and fracture strength is reachable To more than 300MPa.
Embodiment 2
This example molten alloy composition is Mg-7Gd-5Y-2Zn-1.5Nd-0.5Zr-0.4Al.(RE recovery rates are 85%, Zr Recovery rate is 25%, Al recovery rates for 100%, Zn recovery rates are 90%)
1 material prepares
Magnesium-rare earth discard car after deformation is fallen into crust, impurity is reduced.The on-line checking Al content in fusion process, During if fewer than 0.4%, then supplemented according to volume mass.
Raw material is magnesium-rare earth Mg-7Gd-5Y-1.5Nd-0.5Zr waste materials, pure Al, pure Zn;Designing addition is:
The alloy of table 3 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 4.It is to ensure rapid melting, raw material is cut into small pieces, size is being smoothly put into Crucible is defined, and removes surface and oil contaminant, and sand papering removes oxide layer.
The actual raw material addition of the alloy of table 4
2-in-1 golden melting
(1) preheating furnace is warmed up to 350 DEG C and melting furnace is warmed up to 700 DEG C (preheating furnace is resistance furnace, and melting furnace is for can The intermediate frequency electromagnetic induction heater of temperature control), while (being argon gas and 134a gaseous mixtures to protective gas is passed through in above-mentioned two stove Body, the two volume ratio is about 20:1).
A) rare earth EW75 cuttings are blocking, it is ensured that size is close to 3:3:4 (volume ratios), in preheating furnace, by EW75, Al and Zn Ingot is preheating to 350 DEG C, it is ensured that surface is without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.EW75 is put into smelting furnace first, temperature is maintained at 700 DEG C, 20min is incubated after fusing, then skimming;It is put into second block of fritter clout so that clout is completely melt, is incubated 20min, Removal surface scum;The 3rd block of bulk clout is put into, until completely melted, 20min is incubated, is sufficiently stirred for, skimming operation.
C) when adding EW75 to be completely melt slow rising melt temperature simultaneously, when melt temperature is 750 DEG C, 50min will be preheated Zn ingots add, wait to be completely dissolved.
D) at 800 DEG C, particle diameter is 1 centimetre of size to melt temperature when Al is added.After addition, melt is sufficiently stirred for, at 800 DEG C Insulation 30min.On-line period, carries out composition test, less than default content(0.4%), so keeping melt at 800 DEG C, continue to add Plus a small amount of Al, it is 0.4% that on-line period measures Al content again, meets and requires, is then cooled to 750 DEG C.
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 150rad/min, ultrasonic power 10kW).Now melt temperature is maintained at 800 DEG C.Action time is in 50min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 650 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 200mm of extruded barses, and extruder outlet speed is 20mm/s.
4 Homogenization Treatments
Then the bar after extruding is put into the homogenization heat-treatment furnace for having heated up in advance, homogenization temperature is 500 DEG C, Soaking time is in 8h.
5 redeformations
2 multiway forgings are directly carried out after homogenization, is not lowered the temperature in deformation process, maintain the temperature at 500 DEG C, every time forging Insulation 30min is melted down afterwards, then carries out roll forming.
6 coolings and pre-stretching treatment
By the alloy after roll forming directly in 150 DEG C of recyclable quenching oil quenchings coolings, when material temperature with quench Taken out when fiery medium temperature is consistent.
7 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 150 DEG C, when Between be 100h.To after the time, air cooling is taken out.
The alloy for obtaining has applied at elevated temperature performance very high, stabilization can be used at 300 DEG C, and fracture strength can reach More than 230MPa.
Embodiment 3
This example molten alloy composition is Mg-8Gd-4Y-3Zn-1Nd-0.6Zr-0.7Al.(RE recovery rates are received for 85%, Zr Yield is 25%, Al recovery rates for 100%, Zn recovery rates are 90%)
1 material prepares
Zr is got the raw materials ready with Mg-Zr intermediate alloys, and in the intermediate alloy, the component content of Zr is 40%, and remaining is Mg;The Mg in intermediate alloy Mg-Zr is removed, the Mg in remaining magnesium alloy is got the raw materials ready with pure magnesium ingot;Gd, Y, Nd are with proof gold Category form is added, and design addition is:
The alloy of table 5 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 6.It is to ensure rapid melting, raw material is cut into small pieces, size is being smoothly put into Crucible is defined, and removes surface and oil contaminant, and sand papering removes oxide layer.
The actual raw material addition of the alloy of table 6
2-in-1 golden melting
(1) preheating furnace is warmed up to 380 DEG C, and melting furnace is warmed up into 780 DEG C, and (preheating furnace is resistance furnace, and melting furnace is The intermediate frequency electromagnetic induction heater of controllable temperature), while (being that argon gas and 134a mix to protective gas is passed through in above-mentioned two stove Gas, the two volume ratio is about 20:1);
A) in preheating furnace, pure magnesium ingot is preheating to 380 DEG C, continues 15min, it is ensured that in addition will without steam on magnesium ingot surface Rare earth metal, Al, Zn and Mg-Zr intermediate alloy are preheating to same temperature, sequencing are now should be noted that, in general Mg-Zr Between alloy should be preheated finally, and ensure surface without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.To account for first total amount 50% it is preheated after pure magnesium ingot It is put into smelting furnace, it is completely melt under the protection of protective gas, be subsequently adding remaining magnesium ingot, whole process is by temperature control System keeps 10min at 700 DEG C under this state, stirs and exclude scum silica frost.
C) when adding magnesium ingot to be completely melt slow rising melt temperature simultaneously, Gd, Y pure rare-earth metals of 60min will first be preheated Ingot adds melt, and the temperature of melt is 800 DEG C when adding rare earth;Rare earth is completely dissolved as rear, raises melt temperature to 820 DEG C, The Mg-Zr intermediate alloys of 60min will be preheated, will be submerged in melt together with the charging basket for holding them, and wait to be completely dissolved.
D) it is 1 centimetre of Al of size particle diameter to be added when melt temperature is at 820 DEG C.After addition, melt is sufficiently stirred for.Then The Zn that will be preheated is added in melt, is sufficiently stirred for, and subsequently ensures that fluid temperature at 850 DEG C, is incubated 30min, is then cooled to 750 ℃。
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 100rad/min, ultrasonic power 7kW).Now melt temperature is maintained at 800 DEG C.Action time is in 40min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 610 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 150mm of extruded barses, extruder outlet speed 15mm/s.
4 Homogenization Treatments
Material tapping temperature is controlled at 510 DEG C, is then placed in the homogenization heat-treatment furnace for having heated up in advance, homogenization temperature 510 DEG C of degree, soaking time is in 40h.
5 redeformations
Carry out multiway forging direct 4 times after homogenization, do not lower the temperature in deformation process, maintain the temperature at 510 DEG C, between every time Insulation 60min is melted down after forging, last a time forges direct forming.
6 coolings and pre-stretching treatment
The alloy that direct forming will be forged directly is cooled down in recyclable 100 DEG C of quenching oil, when material temperature with quench Taken out when fiery medium temperature is consistent.
7 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 200 DEG C, when Between be 12h.To after the time, air cooling is taken out.
The alloy that deformation is obtained has applied at elevated temperature performance very high, stabilization can be used at 250 DEG C, and fracture strength is reachable To more than 300MPa.
Embodiment 4
This example molten alloy composition is Mg-10Gd-5.5Y-4Zn-1.5Nd-0.9Zr-1Al.(RE recovery rates are 85%, Zr recovery rates are that 25%, Al recovery rates are that 100%, Zn recovery rates are 90%)
1 material prepares
The discard car of the magnesium-rare earth Mg-10Gd-5.5Y-1.5Nd-0.9Zr after deformation is fallen into crust, impurity is reduced. The on-line checking Al content in fusion process, during if fewer than 0.4%, is then supplemented according to volume mass.
Raw material is magnesium-rare earth Mg-10Gd-5.5Y-1.5Nd-0.9Zr waste materials, pure Al, pure Zn;Designing addition is:
The alloy of table 7 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 8.It is to ensure rapid melting, raw material is cut into small pieces, size is being smoothly put into Crucible is defined, and removes surface and oil contaminant, and sand papering removes oxide layer.
The actual raw material addition of the alloy of table 8
2-in-1 golden melting
(1) preheating furnace is warmed up to 400 DEG C and melting furnace is warmed up to 900 DEG C (preheating furnace is resistance furnace, and melting furnace is for can The intermediate frequency electromagnetic induction heater of temperature control), while (being argon gas and 134a gaseous mixtures to protective gas is passed through in above-mentioned two stove Body, the two volume ratio is about 20:1);
A) rare earth Mg-10Gd-5.5Y-1.5Nd-0.9Zr cuttings are blocking, it is ensured that size is close to 3:3:4 (volume ratios), pre- In hot stove, Mg-10Gd-5.5Y-1.5Nd-0.9Zr is preheating to 400 DEG C, preheating time 40min;Al and Zn ingots are equally preheated To 400 DEG C, it is ensured that surface is without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.Mg-10Gd-5.5Y-1.5Nd-0.9Z is put into first In smelting furnace, fritter clout is put into crucible, now furnace temperature is 800 DEG C, 35min is incubated after fusing, then skimming;It is put into Two blocks of fritter clouts so that clout is completely melt that insulation 35min removes surface scum;The 3rd block of bulk clout is put into, has been treated After running down, 35min is incubated, be sufficiently stirred for, skimming operation.
C) when plus Mg-10Gd-5.5Y-1.5Nd-0.9Z be completely melt simultaneously slow to raise melt temperature, melt temperature liter Zn ingots to addition preheating 40min at 900 DEG C high, wait to be completely dissolved.
D) keep melt temperature at 900 DEG C, the particle diameter for adding preheating 20min is 1 centimetre of Al block of size;After addition, fill Divide stirring melt, 30min are incubated at 900 DEG C, on-line period carries out composition test, and then the satisfactory contents of Al are cooled to 750℃。
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 150rad/min, ultrasonic power 10kW).Now melt temperature is maintained at 900 DEG C.Action time is in 50min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 650 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 200mm of extruded barses, and extruder outlet speed is 20mm/s.
4 Homogenization Treatments
Tapping temperature is 510 DEG C, is then put into the bar after extruding in the homogenization heat-treatment furnace for having heated up in advance, Temperature is homogenized for 540 DEG C, soaking time is in 48h.
5 redeformations
5 multiway forgings are directly carried out after homogenization, roll forming is then carried out.Do not lower the temperature in deformation process, keep temperature Degree melts down insulation 100min every time at 550 DEG C after forging, using after the alloy last time multiway forging that multiway forging shapes Do not melt down.
6 coolings and pre-stretching treatment
Alloy after deformation is directly cooled down in 150 DEG C of recyclable quenching oils, when material temperature and hardening media temperature Taken out when spending consistent.
7 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 170 DEG C, when Between be 75h.To after the time, air cooling is taken out.
The alloy that deformation is obtained has applied at elevated temperature performance very high, stabilization can be used at 300 DEG C, and fracture strength is reachable To more than 250MPa.
Embodiment 5
This example molten alloy composition is Mg-12.0Gd-4.5Y-3Zn-0.6Nd-0.4Zr-0.5Al.(RE recovery rates are 85%, Zr recovery rate are that 25%, Al recovery rates are that 100%, Zn recovery rates are 90%)
1 material prepares
Zr is got the raw materials ready with Mg-Zr intermediate alloys, and in the intermediate alloy, the component content of Zr is 30%, and remaining is Mg;The Mg in intermediate alloy Mg-Zr is removed, the Mg in remaining magnesium alloy is got the raw materials ready with pure magnesium ingot;Gd, Y, Nd are with proof gold Category form is added, and design addition is:
The alloy of table 9 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 10.It is to ensure rapid melting, raw material is cut into small pieces, size is smoothly putting Enter crucible to be defined, remove surface and oil contaminant, sand papering removes oxide layer.
The actual raw material addition of the alloy of table 10
2-in-1 golden melting
(1) preheating furnace is warmed up to 370 DEG C, and melting furnace is warmed up into 760 DEG C, and (preheating furnace is resistance furnace, and melting furnace is The intermediate frequency electromagnetic induction heater of controllable temperature), while (being that argon gas and 134a mix to protective gas is passed through in above-mentioned two stove Gas, the two volume ratio is about 20:1);
A) in preheating furnace, pure magnesium ingot is preheating to 370 DEG C, continues 20min, it is ensured that in addition will without steam on magnesium ingot surface Rare earth metal, Al, Zn and Mg-Zr intermediate alloy are preheating to same temperature, sequencing are now should be noted that, in general Mg-Zr Between alloy should be preheated finally, and ensure surface without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.To account for first total amount 50% it is preheated after pure magnesium ingot It is put into smelting furnace, it is completely melt under the protection of protective gas, be subsequently adding remaining magnesium ingot, whole process is by temperature control System keeps 7min at 760 DEG C under this state, stirs and exclude scum silica frost.
C) when adding magnesium ingot to be completely melt slow rising melt temperature simultaneously, Gd, Y pure rare earth that will successively preheat 50mind are golden Category ingot, preheat 40min Mg-Zr intermediate alloys together with hold they charging basket submerged successively according to sequencing magnesium melt In liquid, premised on the two interval time is completely dissolved by rare earth, the temperature of melt is 820 DEG C when adding rare earth, in addition Mg-Zr Between alloy when melt temperature at 850 DEG C.
D) particle diameter of preheating, at 870 DEG C, is that 1 centimetre of Al of size is added by adjustment melt temperature until completely dissolved; After addition, melt is sufficiently stirred for, the Zn that then will be preheating to is added in melt, is sufficiently stirred for, and subsequently ensures that fluid temperature 870 DEG C, 30min is incubated, then it is cooled to 750 DEG C.
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 120rad/min, ultrasonic power 5kW).Now melt temperature is maintained at 800 DEG C.Action time is in 30min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 610 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 80mm of extruded barses, extruder outlet speed 12mm/s.
4 Homogenization Treatments
Material tapping temperature is controlled at 500 DEG C, is then placed in the homogenization heat-treatment furnace for having heated up in advance, homogenization temperature 530 DEG C of degree, soaking time is in 18h.
5 redeformations
Secondary extrusion is directly carried out after homogenization, extrusion temperature is 530 DEG C, and extrusion speed is 15mm/min, extrusion speed It is in inverse ratio with extrusion ratio, extrusion ratio is 4.
6 coolings and pre-stretching treatment
Alloy after deformation is directly cooled down in recyclable 85 DEG C of coolant, when material temperature and hardening media temperature Taken out when spending consistent, carry out pre-stretching treatment, elimination residual stress is simultaneously orthopedic, and pre-stretching amount is 3%.
7 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 225 DEG C, when Between be 32h.To after the time, air cooling is taken out.
The alloy that deformation is obtained has applied at elevated temperature performance very high, stabilization can be used at 250 DEG C, and fracture strength is reachable To more than 300MPa.
Embodiment 6
This example molten alloy composition is Mg-15.0Gd-5.5Y-2.5Zn-1.2Nd-0.3Zr-0.9Al.(RE recovery rates It is that 85%, Zr recovery rates are that 25%, Al recovery rates are that 100%, Zn recovery rates are 90%)
1 material prepares
The discard car of the magnesium-rare earth Mg-6.5Gd-5.5Y-1.2Nd-0.3Zr after deformation is fallen into crust, impurity is reduced. The on-line checking Al content in fusion process, during if fewer than 0.4%, is then supplemented according to volume mass.
Raw material is magnesium-rare earth Mg-6.5Gd-5.5Y-1.2Nd-0.3Zr waste materials, pure Al, pure Zn;Designing addition is:
The alloy of table 11 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 12.It is to ensure rapid melting, raw material is cut into small pieces, size is smoothly putting Enter crucible to be defined, remove surface and oil contaminant, sand papering removes oxide layer.
The actual raw material addition of the alloy of table 12
2-in-1 golden melting
(1) preheating furnace is warmed up to 360 DEG C and melting furnace is warmed up to 730 DEG C (preheating furnace is resistance furnace, and melting furnace is for can The intermediate frequency electromagnetic induction heater of temperature control), while (being argon gas and 134a gaseous mixtures to protective gas is passed through in above-mentioned two stove Body, the two volume ratio is about 20:1);
A) rare earth Mg-6.5Gd-5.5Y-1.2Nd-0.3Zr cuttings are blocking, it is ensured that size is close to 3:3:4 (volume ratios), In preheating furnace, Mg-6.5Gd-5.5Y-1.2Nd-0.3Zr is preheating to 360 DEG C, preheating time 25min;Al and Zn ingots is same It is preheating to 360 DEG C, it is ensured that surface is without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.Mg-6.5Gd-5.5Y-1.2Nd-0.3Zr is put first Enter in smelting furnace, fritter clout is put into crucible, be warming up to 800 DEG C, 35min is incubated after fusing, then skimming;It is put into second Block fritter clout so that clout is completely melt that insulation 35min removes surface scum;The 3rd block of bulk clout is put into, is treated completely After fusing, 35min is incubated, be sufficiently stirred for, skimming operation.
C) when adding Mg-6.5Gd-5.5Y-1.2Nd-0.3Zr to be completely melt slow rising melt temperature simultaneously, by 40min's Zn adds melt when melt temperature is 780 DEG C together with the charging basket for holding them, waits to be completely dissolved.
D) it is that 1 centimetre of Al of size adds melt by the particle diameter of preheating when melt temperature is at 810 DEG C;After addition, fully Stirring melt, 30min is incubated at 810 DEG C, and on-line period carries out composition test, meets default Al content, is then cooled to 750 ℃。
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 75rad/min, ultrasonic power 4kW).Now melt temperature is maintained at 810 DEG C.Action time is in 45min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 620 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 30mm of extruded barses, and extruder outlet speed is 6mm/s.
4 coolings and pre-stretching treatment
Alloy after deformation is directly cooled down in 90 DEG C of recyclable quenching oils, when material temperature and hardening media temperature Taken out when consistent, carry out amount of tension for 4% pre-stretching is processed, elimination residual stress is simultaneously orthopedic.
7 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 180 DEG C, when Between be 50h.To after the time, air cooling is taken out.
The alloy that deformation is obtained has applied at elevated temperature performance very high, stabilization can be used at 280 DEG C, and fracture strength is reachable To more than 280MPa.
Embodiment 7
This example molten alloy composition is Mg-9Gd-5Y-2.5Zn-0.5Nd-0.8Zr-0.6Al.(RE recovery rates are 85%, Zr recovery rates are that 25%, Al recovery rates are that 100%, Zn recovery rates are 90%)
1 material prepares
Zr is got the raw materials ready with Mg-Zr intermediate alloys, and in the intermediate alloy, the component content of Zr is 30%, and remaining is Mg;The Mg in intermediate alloy Mg-Zr is removed, the Mg in remaining magnesium alloy is got the raw materials ready with pure magnesium ingot;Gd、Y、Nd、Zn、Al Added with form of pure metal, design addition is:
The alloy of table 13 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 14.It is to ensure rapid melting, raw material is cut into small pieces, size is smoothly putting Enter crucible to be defined, remove surface and oil contaminant, sand papering removes oxide layer.
The actual raw material addition of the alloy of table 14
2-in-1 golden melting
(1) preheating furnace is warmed up to 320 DEG C, and melting furnace is warmed up into 650 DEG C, and (preheating furnace is resistance furnace, and melting furnace is The intermediate frequency electromagnetic induction heater of controllable temperature), while (being that argon gas and 134a mix to protective gas is passed through in above-mentioned two stove Gas, the two volume ratio is about 20:1);
A) in preheating furnace, pure magnesium ingot is preheating to 350 DEG C, continues 15min, it is ensured that in addition will without steam on magnesium ingot surface Rare earth metal, Al, Zn and Mg-Zr intermediate alloy are preheating to same temperature, sequencing are now should be noted that, in general Mg-Zr Between alloy should be preheated finally, and ensure surface without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.To account for first total amount 50% it is preheated after pure magnesium ingot It is put into smelting furnace, it is completely melt under the protection of protective gas, be subsequently adding remaining magnesium ingot, whole process is by temperature control System keeps 10min at 750 DEG C under this state, stirs and exclude scum silica frost.
C) when adding magnesium ingot to be completely melt slow rising melt temperature simultaneously, Gd, Y pure rare earth that will successively preheat 45min are golden Category ingot, preheat 55min Mg-Zr intermediate alloys together with hold they charging basket submerged successively according to sequencing magnesium melt In liquid, premised on the two interval time is completely dissolved by rare earth, the temperature of melt is 850 DEG C when adding rare earth, in addition Mg-Zr Between alloy when melt temperature also at 850 DEG C.
D) particle diameter of preheating, at 850 DEG C, is that 1 centimetre of Al of size is added by adjustment melt temperature until completely dissolved; After addition, melt is sufficiently stirred for, the Zn that then will be preheating to is added in melt, is sufficiently stirred for, and subsequently ensures that fluid temperature 850 DEG C, 30min is incubated, then it is cooled to 750 DEG C.
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 140rad/min, ultrasonic power 8kW).Now melt temperature is maintained at 780 DEG C.Action time is in 40min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 650 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 180mm of extruded barses, extruder outlet speed 16mm/s.
4 Homogenization Treatments
Material tapping temperature is controlled at 490 DEG C, is then placed in the homogenization heat-treatment furnace for having heated up in advance, homogenization temperature 525 DEG C of degree, soaking time is in 45h.
5 redeformations
Multiway forging is carried out after homogenization direct 4 times, then carry out direct forging and molding.Do not lower the temperature in deformation process, protect Temperature is held at 500 DEG C, between every time forging after melt down insulation 70min, do not melted down after last forging and molding.
6 coolings and pre-stretching treatment
Alloy after deformation is directly cooled down in recyclable 120 DEG C of quenching oil, when material temperature and hardening media Taken out when temperature is consistent.
7 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 200 DEG C, when Between be 55h.To after the time, air cooling is taken out.
The alloy that deformation is obtained has applied at elevated temperature performance very high, stabilization can be used at 250 DEG C, and fracture strength is reachable To more than 300MPa.
Embodiment 8
This example molten alloy composition is Mg-7.5Gd-4.5Y-3Zn-0.9Nd-0.4Zr-0.7Al.(RE recovery rates are 85%, Zr recovery rate are that 25%, Al recovery rates are that 100%, Zn recovery rates are 90%)
1 material prepares
The discard car of the magnesium-rare earth Mg-7.5Gd-4.5Y-0.9Nd-0.4Zr after deformation is fallen into crust, impurity is reduced. The on-line checking Al content in fusion process, during if fewer than 0.4%, is then supplemented according to volume mass.
Raw material is magnesium-rare earth Mg-7.5Gd-4.5Y-0.9Nd-0.4Zr waste materials, pure Al, pure Zn;Designing addition is:
The alloy of table 15 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 16.It is to ensure rapid melting, raw material is cut into small pieces, size is smoothly putting Enter crucible to be defined, remove surface and oil contaminant, sand papering removes oxide layer.
The actual raw material addition of the alloy of table 16
2-in-1 golden melting
(1) preheating furnace is warmed up to 380 DEG C and melting furnace is warmed up to 790 DEG C (preheating furnace is resistance furnace, and melting furnace is for can The intermediate frequency electromagnetic induction heater of temperature control), while (being argon gas and 134a gaseous mixtures to protective gas is passed through in above-mentioned two stove Body, the two volume ratio is about 20:1);
A) rare earth Mg-7.5Gd-4.5Y-0.9Nd-0.4Zr cuttings are blocking, it is ensured that size is close to 3:3:4 (volume ratios), In preheating furnace, Mg-7.5Gd-4.5Y-0.9Nd-0.4Zr is preheating to 380 DEG C, preheating time 30min;Al and Zn ingots is same It is preheating to 380 DEG C, it is ensured that surface is without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.Mg-7.5Gd-4.5Y-0.9Nd-0.4Zr is put first Enter in smelting furnace, fritter clout is put into crucible, be warming up to 800 DEG C, 25min is incubated after fusing, then skimming;It is put into second Block fritter clout so that clout is completely melt that insulation 20min removes surface scum;The 3rd block of bulk clout is put into, is treated completely After fusing, 15min is incubated, be sufficiently stirred for, skimming operation.
C) when adding Mg-7.5Gd-4.5Y-0.9Nd-0.4Zr to be completely melt slow rising melt temperature simultaneously, by 30min's Zn adds melt when melt temperature is 820 DEG C together with the charging basket for holding them, waits to be completely dissolved.
D) it is that 1 centimetre of Al of size adds melt by the particle diameter of preheating when melt temperature is at 820 DEG C;After addition, fully Stirring melt, 30min is incubated at 820 DEG C, and on-line period carries out composition test, meets default Al content, is then cooled to 750 ℃。
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 130rad/min, ultrasonic power 10kW).Now melt temperature is maintained at 800 DEG C.Action time is in 30min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 620 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 10mm of extruded barses, and extruder outlet speed is 5mm/s.
4 coolings and pre-stretching treatment
Alloy after deformation is directly cooled down in 85 DEG C of recyclable coolants, when material temperature and hardening media temperature Taken out when consistent, carry out the pre-stretching treatment that amount of tension is 2%, elimination residual stress is simultaneously orthopedic.
5 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 250 DEG C, when Between be 8h.To after the time, air cooling is taken out.
The alloy that deformation is obtained has applied at elevated temperature performance very high, stabilization can be used at 250 DEG C, and fracture strength is reachable To more than 300MPa, while having good creep-resistant property.
Embodiment 9
This example molten alloy composition is Mg-8Gd-5Y-2Zn-0.5Nd-0.8Zr-1Al.(RE recovery rates are received for 85%, Zr Yield is 25%, Al recovery rates for 100%, Zn recovery rates are 90%)
1 material prepares
Zr is got the raw materials ready with Mg-Zr intermediate alloys, and in the intermediate alloy, the component content of Zr is 30%, and remaining is Mg;The Mg in intermediate alloy Mg-Zr is removed, the Mg in remaining magnesium alloy is got the raw materials ready with pure magnesium ingot;Gd、Y、Nd、Zn、Al Added with form of pure metal, design addition is:
The alloy of table 17 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 18.It is to ensure rapid melting, raw material is cut into small pieces, size is smoothly putting Enter crucible to be defined, remove surface and oil contaminant, sand papering removes oxide layer.
The actual raw material addition of the alloy of table 18
2-in-1 golden melting
(1) preheating furnace is warmed up to 300 DEG C, and melting furnace is warmed up into 650 DEG C, and (preheating furnace is resistance furnace, and melting furnace is The intermediate frequency electromagnetic induction heater of controllable temperature), while (being that argon gas and 134a mix to protective gas is passed through in above-mentioned two stove Gas, the two volume ratio is about 20:1);
A) in preheating furnace, pure magnesium ingot is preheating to 300 DEG C, continues 15min, it is ensured that in addition will without steam on magnesium ingot surface Rare earth metal, Al, Zn and Mg-Zr intermediate alloy are preheating to same temperature, sequencing are now should be noted that, in general Mg-Zr Between alloy should be preheated finally, and ensure surface without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.To account for first total amount 50% it is preheated after pure magnesium ingot It is put into smelting furnace, it is completely melt under the protection of protective gas, be subsequently adding remaining magnesium ingot, whole process is by temperature control System keeps 10min at 720 DEG C under this state, stirs and exclude scum silica frost.
C) when adding magnesium ingot to be completely melt slow rising melt temperature simultaneously, Gd, Y pure rare earth that will successively preheat 40min are golden Category ingot, preheat 50min Mg-Zr intermediate alloys together with hold they charging basket submerged successively according to sequencing magnesium melt In liquid, premised on the two interval time is completely dissolved by rare earth, the temperature of melt is 820 DEG C when adding rare earth, in addition Mg-Zr Between alloy when melt temperature at 850 DEG C.
D) particle diameter of preheating, at 880 DEG C, is that 1 centimetre of Al of size is added by adjustment melt temperature until completely dissolved; After addition, melt is sufficiently stirred for, then will be preheating in Zn addition melts, be sufficiently stirred for, subsequently ensure that fluid temperature 830 DEG C, 30min is incubated, then it is cooled to 750 DEG C.
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 60rad/min, ultrasonic power 10kW).Now melt temperature is maintained at 770 DEG C.Action time is in 45min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 600 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 200mm of extruded barses, extruder outlet speed 20mm/s.
4 Homogenization Treatments
Material tapping temperature is controlled at 510 DEG C, is then placed in the homogenization heat-treatment furnace for having heated up in advance, homogenization temperature 515 DEG C of degree, soaking time is in 30h.
5 redeformations
Multiway forging is carried out after homogenization direct 3 times, then carry out extrusion molding.Do not lower the temperature in deformation process, keep temperature Degree at 550 DEG C, between every time forging after melt down insulation 30min;The extrusion molding that extrusion ratio is 5 is carried out after multiway forging.
6 coolings and pre-stretching treatment
Alloy after extrusion molding is directly cooled down in recyclable 120 DEG C of quenching oil, when material temperature and quenching Taken out when medium temperature is consistent, carry out the pre-stretching treatment that amount of tension is 5%, elimination residual stress is simultaneously orthopedic.
7 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 205 DEG C, when Between be 50h.To after the time, air cooling is taken out.
The alloy that deformation is obtained has applied at elevated temperature performance very high, stabilization can be used at 250 DEG C, and fracture strength is reachable To more than 300MPa, while having good creep-resistant property.
Embodiment 10
This example molten alloy composition is Mg-9Gd-3Y-3.5Zn-1.2Nd-0.8Zr-0.6Al.(RE recovery rates are 85%, Zr recovery rates are that 25%, Al recovery rates are that 100%, Zn recovery rates are 90%)
1 material prepares
The discard car of the magnesium-rare earth Mg-9Gd-3.5Y-1.2Nd-0.8Zr after deformation is fallen into crust, impurity is reduced. On-line checking Al content in fusion process, during if fewer than 0.4%, is then supplemented according to volume mass.
Raw material is magnesium-rare earth Mg-9Gd-3.5Y-1.2Nd-0.8Zr waste materials, pure Al, pure Zn;Designing addition is:
The alloy of table 19 designs component list(wt.%)
According to experiment material consumption and crucible size, this experimental design melting 100kg, it is considered to which alloying element is damaged during melting Lose, design alloying component and raw material addition are shown in Table 20.It is to ensure rapid melting, raw material is cut into small pieces, size is smoothly putting Enter crucible to be defined, remove surface and oil contaminant, sand papering removes oxide layer.
The actual raw material addition of the alloy of table 20
2-in-1 golden melting
(1) preheating furnace is warmed up to 350 DEG C and melting furnace is warmed up to 770 DEG C (preheating furnace is resistance furnace, and melting furnace is for can The intermediate frequency electromagnetic induction heater of temperature control), while (being argon gas and 134a gaseous mixtures to protective gas is passed through in above-mentioned two stove Body, the two volume ratio is about 20:1);
A) rare earth Mg-9Gd-3.5Y-1.2Nd-0.8Zr cuttings are blocking, it is ensured that size is close to 3:3:4 (volume ratios), pre- In hot stove, Mg-9Gd-3.5Y-1.2Nd-0.8Zr is preheating to 350 DEG C, preheating time 35min;Al and Zn ingots are equally preheated To 350 DEG C, it is ensured that surface is without steam.
B) alloy melting is carried out in the smelting furnace having been warmed up.Mg-9Gd-3.5Y-1.2Nd-0.8Zr is put into first In smelting furnace, fritter clout is put into crucible, is warming up to 800 DEG C, 40min is incubated after fusing, then skimming;It is put into second piece Fritter clout so that clout is completely melt that insulation 30min removes surface scum;The 3rd block of bulk clout is put into, treats to melt completely After change, 20min is incubated, be sufficiently stirred for, skimming operation.
C) when adding Mg-9Gd-3.5Y-1.2Nd-0.8Zr to be completely melt slow rising melt temperature simultaneously, by the Zn of 35min Melt is added together with the charging basket for holding them when melt temperature is 810 DEG C, waits to be completely dissolved.
D) it is that 1 centimetre of Al of size adds melt by the particle diameter of preheating when melt temperature is at 840 DEG C;After addition, fully Stirring melt, 30min is incubated at 820 DEG C, and on-line period carries out composition test, meets default Al content, is then cooled to 750 ℃。
(2) physical field stirring
Be slowly added to ultrasonic device and agitating device, allow mechanical agitation and it is ultrasonically treated at the same act on melt (machinery Speed of agitator 120rad/min, ultrasonic power 9kW).Now melt temperature is maintained at 790 DEG C.Action time is in 45min.
3 alloy semi-solids are extruded
After stirring, all mechanisms are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, be cooled to 610 DEG C, protected Warm 10min, carries out semi-solid state extrusion, a diameter of 80mm of extruded barses, and extruder outlet speed is 7mm/s.
4 Homogenization Treatments
Extrded material tapping temperature is controlled at 500 DEG C, is then placed in the homogenization heat-treatment furnace for having heated up in advance, uniformly It is 540 DEG C, soaking time 46h to change temperature.
5 redeformations
Bar directly carries out secondary extrusion, and extrusion temperature is 540 DEG C, and extrusion speed is 12mm/min, and extrusion ratio is 15.
6 coolings and pre-stretching treatment
Alloy after deformation is directly cooled down in 85 DEG C of recyclable quenching oils, when material temperature and hardening media temperature Taken out when consistent, carry out the pre-stretching treatment that amount of tension is 3%, elimination residual stress is simultaneously orthopedic.
7 ageing strengthenings are processed
Material with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is 160 DEG C, when Between be 85h.To after the time, air cooling is taken out.
The alloy that deformation is obtained has applied at elevated temperature performance very high, stabilization can be used at 250 DEG C, and fracture strength is reachable To more than 300MPa, while having good creep-resistant property.
The present invention take full advantage of Al preferentially with alloy in rare earth and Zr formed stable phase shortcoming, auxiliary with the addition of Zn Unit usually compensates its defect, and is prepared for being improve with high performance wrought magnesium alloy the recovering effect of rare earth element, while will Semi-solid-state shaping is combined with solid plastics shaping, and the alloy developed has room temperature and mechanical behavior under high temperature higher, Particularly prominent creep-resistant property.

Claims (10)

1. a kind of rare earth wrought magnesium alloy containing minor-alloying element Al, its percentage by weight composition is:Gd:6.5~15.0%, Y: 3.0~5.5%, Zn:2.0~4.0%, Nd:0.3~1.5%, Zr:0.3~0.9%, Al:0.4~1.0%, balance of Mg.
2. the preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al described in claim 1, comprises the following steps:
(1) raw material prepares
Got the raw materials ready by the percentage by weight of described magnesium alloy composition;Or using the magnesium-rare earth discard after deformation, warp Composition test is crossed, Al and/or Zn is added;
(2) alloy melting
Preheating furnace is warmed up to 300 DEG C~400 DEG C, and melting furnace is warmed up to 600 DEG C~900 DEG C, while to above-mentioned two stove Protective gas is passed through in son;After raw material is preheated in the preheating furnace respectively, being added in the smelting furnace of preheating carries out alloy melting, extremely After being completely melt, ultrasonic device and agitating device are added, mechanical agitation and ultrasonically treated is carried out to liquation;
(3) alloy semi-solid extruding
After stirring, mechanical agitation and ultrasonic processing apparatus are all taken out, liquation is poured into the chamber of semi-solid state extrusion machine, is lowered the temperature To 600 DEG C~650 DEG C, 10min is incubated, semi-solid state extrusion is carried out, between a diameter of 10mm~200mm of extruded barses;
(4) cooling and pre-stretching treatment
Alloy after deformation is cooled down in 80 DEG C~150 DEG C recyclable hardening medias, when bar temperature and hardening media temperature Taken out when spending consistent;The bar for shaping carries out pre-stretching treatment, and elimination residual stress is simultaneously orthopedic, and pre-tension deformation amount is 2 ~5%;
(5) ageing strengthening treatment
Bar with temperature after quenching is directly placed into aging strengthening model stove and is heat-treated, temperature is at 150 DEG C~250 DEG C Between, the time be 8h~100h between, subsequent air cooling.
3. the preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al according to claim 2, it is characterised in that It is further comprising the steps of after step (3):
(3)-A Homogenization Treatments
By the control of bar tapping temperature at 500 DEG C ± 10 DEG C, it is then placed in the homogenization heat-treatment furnace for having heated up in advance, uniformly Change temperature between 500 DEG C~540 DEG C, soaking time is in 8h~48h;
(3)-B1 redeformations
Secondary extrusion is carried out, extrusion temperature is homogenization temperature, and extrusion speed is 5mm~15mm/min, extrusion speed and extruding Than in inverse ratio, extrusion ratio controlled quentity controlled variable is 4~25.
4. the preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al according to claim 2, it is characterised in that It is further comprising the steps of after step (3):
(3)-A Homogenization Treatments
By the control of bar tapping temperature at 500 DEG C ± 10 DEG C, it is then placed in the homogenization heat-treatment furnace for having heated up in advance, uniformly Change temperature between 500 DEG C~540 DEG C, soaking time is in 8h~48h;
(3)-B2 redeformations
2~5 multiway forgings are carried out after homogenization, is not lowered the temperature in deformation process, maintain the temperature at 500 DEG C~550 DEG C, every time forging Insulation 30min~100min is melted down after making, is then extruded, rolled or direct forging and molding.
5. the preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al according to any one of claim 2-4, its It is characterised by:Zr is added in Mg-Zr intermediate alloys form, in described Mg-Zr intermediate alloys, the component content of Zr for 30~ 40wt%;Other alloying elements are added with form of pure metal.
6. the preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al according to claim 5, it is characterised in that:Press It is that 85%, Zr recovery rates are that 25%, Al recovery rates are that 100%, Zn recovery rates are 90% according to rare earth metal recovery rate, calculates alloy The addition weight of element.
7. the preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al according to any one of claim 2-4, its It is characterised by:Described preheating furnace is resistance furnace, and described melting furnace is the intermediate frequency electromagnetic induction heater of controllable temperature;Described Protective gas is argon gas and 134a mixed gas, and the two volume ratio is 20:1.
8. the preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al according to any one of claim 2-4, its It is characterised by:To account for first gross weight 50% it is preheated after pure magnesium ingot be put into smelting furnace, remaining magnesium is added after being completely melt Ingot, period temperature control keeps 5min~10min at 660 DEG C~720 DEG C, stirs and exclude scum silica frost;After magnesium ingot is completely melt It is slow to raise melt temperature, the rare earth metal of preheating is added, ensure that the temperature of melt is not less than 750 DEG C during addition;When in melt Rare earth metal slow Mg-Zr intermediate alloys for raising melt temperature, adding preheating after dissolving completely, ensure melt temperature during addition Between 800 DEG C~850 DEG C;The Al of preheating is added, melt temperature is sufficiently stirred for melt more than 800 DEG C during addition, 800 DEG C of insulation 30min, are then cooled to 750 DEG C;Zn is added, is sufficiently stirred for, it is ensured that fluid temperature is not less than 750 DEG C.
9. the preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al according to any one of claim 2-4, its It is characterised by:Magnesium-rare earth clout cutting after deformation is blocking, and volume ratio is close to 3:3:4, its composition meets quality percentage Than for:Mg- (6.5~15.0) Gd- (3.0~5.5) Y- (0.3~1.5) Nd- (0.3~0.9) Zr, under a shielding gas together Preheated, the time is 20min~40min;One fritter clout is put into crucible, 600 DEG C~800 DEG C, after fusing are warming up to Insulation 20min~40min, then skimming;It is put into second block of fritter clout so that clout is completely melt, insulation 20min~ 40min, removes surface scum;The 3rd block of bulk clout is put into, until completely melted, 20min~40min is incubated, is sufficiently stirred for, Skimming operation;On-line period, carries out composition test, and Al is added when Al constituent contents are less than 0.4%, if meeting composition needs, Subsequent step is then carried out, 750 DEG C are then cooled to;Zn is added, is sufficiently stirred for, now ensure that fluid temperature is not less than 750 DEG C.
10. the preparation method of the rare earth wrought magnesium alloy containing minor-alloying element Al according to any one of claim 2-4, its It is characterised by:Described mechanical agitation rotating speed is 60~150rad/min, and ultrasonic power is 3kW~10kW, and melt temperature keeps Between 750 DEG C -800 DEG C, action time is 20min-50min.
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