CN103290292A - High strength magnesium alloy and preparation method thereof - Google Patents
High strength magnesium alloy and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a high strength magnesium alloy and a preparation method thereof. The magnesium alloy comprises the following components, by mass: 1.0-15.0% of Cd, 2.0-10.0% of Bi, 5.0-13.0% of Zn, 7.0-15.0% of Y, 0.4-1.0% of Zr, 0.1-5.0% of Nb, impurity elements, and the balance of Mg, wherein the total amount of the impurity elements such as Si, Fe, Cu and Ni is less than 0.02%. The preparation method comprises: adopting an electromagnetic semi-continuous casting method to prepare a magnesium alloy ingot billet, sequentially carrying out uniformization annealing and surface turning on the ingot billet, heating, adopting a reverse extrusion device to carry out reverse extrusion on the ingot billet, and carrying out a heat treatment on the extruded rod material. According to the prepared magnesium alloy material, room temperature mechanical properties can be that a tensile strength is 410-450 MPa, a yield strength is 350-380 MPa, and an elongation rate is more than 6%.
Description
Technical field
The invention belongs to metallic substance and metallurgical technology field, be specifically related to a kind of high-strength magnesium alloy and preparation method thereof.
Background technology
The crystalline structure of magnesium alloy belongs to hexagonal close packed lattice, its plastic deformation ability is not as good as aluminium and steel, increase the difficulty of magnesium alloy plastic working and produced preparation cost, for this reason in the novel magnesium alloy development research in recent years, begun to pay attention to design mutually and adopt mode such as new deformation technique by the wrought magnesium alloys interalloy, when guaranteeing certain intensity, more paid attention to improving the plastic working ability of magnesium alloy.
Because it is little that magnesium alloy has density, specific rigidity and specific tenacity height, and excellent heat conductivity performance, capability of electromagnetic shielding, damping capacity, machinability and damping performance arranged, have series of advantages such as dimensional stabilizing, pollution-free, easy recovery simultaneously, be that light in structure quantizes ideal material, in industry such as automobile, aerospace, national defence and 3C Product, wide commercial application prospect arranged.Yet because the magnesium alloy absolute strength is low, the deformation at room temperature ability is relatively poor, and easily oxidizing fire, defective such as perishable have limited its widespread use as structured material, and to can not show a candle to aluminium alloy extensive for Application of Magnesium at present.Therefore, improving magnesium alloy strength and make it have good comprehensive performances, is the novel magnesium alloy hot of research and development, and high-strength magnesium alloy exploitation simultaneously is significant to expanding the Application of Magnesium field.
At present, the Mg-Al-Zn of commercial extensive application system and Mg-Zn-Zr are that alloy maximum intensity after distortion and thermal treatment also is no more than 350MPa, and the magnesium alloy of intensity also is difficult to satisfy the requirement of high performance structures material like this.For improving thermotolerance and the obdurability of magnesium zinc zirconium series magnesium alloy material, researcher has been carried out a large amount of research work, for example people such as Kun Yu has reported that at " Scripta Materialia " 2003 the 48th volumes a kind of novel magnesium zinc zirconium series magnesium alloy Mg-2.8%Ce-0.7%Zn-0.7%Zr (wt.%), this alloy possess the tensile strength of 257.8Mpa and 12% unit elongation at 25 ℃; Patent publication No. is that the Chinese patent of CN101603138A discloses a kind of magnesium zinc zirconium series magnesium alloy Mg-0.2%Y-0.1%Zn-0.6%Zr (wt.% that adds rare earth element yttrium, more excellent proportioning among the embodiment), it at room temperature possesses the tensile strength of 179Mpa and 7.2% unit elongation; Patent publication No. be CN101314829A patent disclosure a kind of quasi crystal phase fortified Mg-Zn-Y-Zr magnesium alloy and preparation method thereof, problems such as magnesium alloy reinforcement have been solved, tensile strength is 290-360MPa, and yield strength is 175-260MPa, and unit elongation is 10-18%; In addition, the applying date is that China's patent " a kind of high plastic magnesium alloy that contains the rare earth yttrium " of on November 11st, 2004, Granted publication CN1297676C discloses a kind of high plastic magnesium alloy that contains the rare earth yttrium, each constituent mass percentage composition is Zn:5.0-8.5%, Zr:0.6-0.8%, Y:0.7-2.0%, tensile strength is 322-337MPa, and yield strength is 263-267MPa, and unit elongation is 18-21%.
Therefore, this two substantially series magnesium alloy be widely used in load assembly and be restricted.And the intensity that wants to improve magnesium alloy can improve alloy strength mutually by adding particle or fiber reinforcement, and it is slight also can to improve alloy by the preparation method of complexity such as strong moulding distortion or powder metallurgy.But above-mentioned two kinds of methods all can't prepare the large size magnesium alloy structural part, so its application is restricted.Adding the alloying element reinforced magnesium alloy is the method that improves a kind of simple efficient and cost-effective practicality of magnesium alloy strength, improves the most general of intensity use by adding a large amount of alloying elements at present in the high-strength magnesium alloy performance history.In the various alloying elements that improve the magnesium alloy performance, strengthening effect was best when multiple rare earth element was united use.At present, the exploitation of high-strength magnesium alloy generally contains two kinds and two or more rare earth element.In addition, rare earth element has purification, degasification and deslagging effect in cast magnesium alloys, can effectively reduce the influence of gas, oxide compound and harmful element.Simultaneously, the part rare earth element can the refinement alloy structure or solid solution diffusion in matrix inside the mechanical property with reinforced magnesium alloy, can also in metal, form rare earth compound, these compounds produce poly-partially at the crystal boundary place of magnesium alloy substrate, and then increased dislocation desity, increase the lattice distortion degree, thereby reached the purpose of reinforcement.Though the adding of a large amount of rare earth elements can improve the intensity of magnesium alloy greatly, the consequent is magnesium alloy materials price comparison height, and high magnesium-rare earth is widely applied and is restricted.Therefore the no rare earth of exploitation or the high-strength magnesium alloy that contains a small amount of rare earth element have great importance.
Summary of the invention
Problem at the prior art existence, the invention provides a kind of high-strength magnesium alloy and preparation method thereof, this processing method cost is low and simple and easy to do, and the magnesium alloy of acquisition has higher intensity, makes this type of magnesium alloy have the mechanical property more superior than conventional commercial magnesium alloy.
A kind of high-strength magnesium alloy provided by the invention, each component and mass percent thereof are: 1.0～15.0% Cd, 2.0～10.0% Bi, 5.0%～13.0% Zn, 7.0%～15.0% Y, 0.4～1.0% Zr, 0.1～5.0% Nb, the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg.
The preparation method of a kind of high-strength magnesium alloy provided by the invention, it mainly comprises following step:
(1) Mg, Cd, Bi, Zn, Y, Nb and Zr are pressed the described ingredient composition of claim 1, wherein Mg, Cd, Bi and Zn add with the form of technical pure Mg, pure Cd, pure Bi and pure Zn, and Y, Nb and Zr add with the form of Mg-25 (or 50) wt.%Y, Zn-30wt.%Nb and Mg-30wt.%Zr master alloy respectively;
(2) place baking oven to carry out preheating respectively raw material in (1) in the claim 1, preheating temperature is 150～200 ℃, and be 2～3h warm up time;
(3) smelting furnace is warming up to 650～750 ℃, the pure Mg of preheating and Mg-Y master alloy are put into smelting furnace to be melted, need to feed shielding gas and insulating covering agent in the melting process, after treating that above-mentioned raw materials all melts, adopt agitator that alloy liquid is stirred 5～10min and make its even mixing, remove the slag on alloy liquid surface then;
(4) above-mentioned alloy liquid is warming up to 720～750 ℃ and adds metal Bi, master alloy stirs after melting fully, adds Mg-Zr and Zn-Nb master alloy in batches after alloy liquid further is warming up to 780～800 ℃, and fully stirs; The alloy liquid temp is down to 720～740 ℃ adds pure Cd and pure Zn, treat that pure Cd and pure Zn melt fully after; Adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 30～60min 700～720 ℃ of insulations and cast;
(5) ingot blank of casting is put into the resistance-type process furnace that has recirculating air and carried out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 500～530 ℃ of insulation 10～15h behind 350～400 ℃ of insulation 5～8h;
(6) ingot blank after the homogenizing is carried out surperficial turning, ingot blank diameter and length are worked into extrusion machine internal diameter of the container and length are complementary; The ingot blank that processes is put into process furnace be heated to 340～420 ℃, insulation 5～10h;
(7) container of the ingot blank that heats being put into prior preheating pushes, and extrusion speed is 1.0～5.0m/min, and the container preheating temperature is 320～400 ℃, and extrusion ratio is 10～50: 1, obtains extruded bars;
(8) extruded bars that obtains is carried out two-stage time effect and handle, its process system is: be warming up to 180～220 ℃ of insulation 30～80h behind 120～160 ℃ of insulation 3～8h, air cooling makes the high-strength magnesium alloy material.
The cunning semi-continuous casting method of low frequency electromagnetic is adopted in described casting, the casting technique system is: electromagnetic field frequency is 20～30Hz, and magneticstrength is 15～30mT, and casting speed is 20～80mm/min, cooling water inflow is 50～400L/min, and crystallizer is wrought aluminium cover crystallizer.
Described shielding gas is SF
6+ CO
2+ Ar mixed gas, SF
6: CO
2: the Ar volume ratio is 0.5: 40: 50.
Compared with prior art, the invention has the beneficial effects as follows:
(1) to compare rare earth element less for high-strength magnesium alloy of the present invention and other high-strength magnesium alloys, and used starting material are easy to obtain, and cost is low, and the cost performance height is easy to scale operation.
(2) technology of the present invention is simple, and equipment used is conventional general-purpose equipment, is easy to transplant and operation, and cost is low, can obviously improve the low problem of alloy strength, can solve magnesium alloy limits its application owing to intensity is a low difficult problem, also can enlarge the Application of Magnesium field.
(3) the magnesium alloy room temperature tensile performance of alloy compositions provided by the invention and method thereof preparation is: tensile strength is 410～450MPa, and yield strength is 350～380MPa, and unit elongation is greater than 6%.
Embodiment
Further specify the present invention below by embodiment.It should be understood that embodiments of the invention are for explanation the present invention rather than limitation of the present invention.Essence according to the present invention all belongs to the scope of protection of present invention to the simple modifications that the present invention carries out.
Mg, Cd, Bi and Zn add with magnesium ingot (99.95%), cadmium ingot (99.99%), bismuth ingot (99.99%) and zinc ingot metal (99.95%) respectively in the present embodiment, Y, Nb and Zr all adopt the form of master alloy to add, and each master alloy is formed massfraction and is respectively: Mg-25 (or 50) %Y, Zn-30%Nb and Mg-30%Zr.
In the present embodiment in the alloy casting process used shielding gas be SF
6+ CO
2+ Ar mixed gas, SF
6: CO
2: the Ar volume ratio is 0.5: 40: 50.
According to the standard of GB GB228-2002, the various magnesium alloy materials of present embodiment gained are carried out the room-temperature mechanical property test.
Embodiment 1:
The composition of alloy (mass percent) is: Cd content is that 10.0%, Bi content is that 5.0%, Zn content is that 5%, Y content is that 7.0%, Zr content is that 0.6%, Nb content is 0.1%, and the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg.In the present embodiment in the alloy melting process used insulating covering agent each component and weight part thereof be 5 gram sulphur, 250 gram diatomite, 200 gram boric acid, silicon sol 45 grams, insulating covering agent accounts for 1.0% of alloy melt gross weight; Refining agent each component and mass percent thereof are 900 gram CaCl
2, 1200 the gram KCl, 150 the gram CaF
2, 750 the gram BaCl
2Mixture, refining agent accounts for 6.0% of alloy melt gross weight.
Weigh up the corresponding ingot metal of total amount 50Kg and master alloy by mentioned component, and load weighted ingot metal and master alloy are put into temperature is that 150 ℃ of baking ovens carry out the preheating of 2h;
Earlier to put into preheating temperature be that 700 ℃ smelting furnace melts for Mg ingot that preheating is good and Mg-25 (or 50) %Y master alloy, need to feed shielding gas and insulating covering agent in the melting process, after treating the above-mentioned raw materials fusing, adopt agitator that alloy liquid is stirred 5min, remove the slag on alloy liquid surface and spread insulating covering agent protected in its surface;
Melt temperature in the smelting furnace is risen to 730 ℃, add metal Bi, master alloy stirs after melting fully, adds Mg-Zr and Zn-Nb master alloy in batches after alloy liquid further is warming up to 780 ℃, and fully stirs; The alloy liquid temp is down to 730 ℃ adds pure Cd and pure Zn, after treating that pure Cd and pure Zn melt fully, adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 50min 710 ℃ of insulations and carry out the cunning semicontinuous casting of low frequency electromagnetic, in castingprocesses, protected with shielding gas; The casting technique system is: electromagnetic field frequency is 30Hz, and magneticstrength is 20mT, and casting speed is 80mm/min, and cooling water inflow is 100L/min, and crystallizer is wrought aluminium cover crystallizer, obtains the ingot blank that diameter is 165mm;
The ingot blank of preparation is put into the resistance-type process furnace that has recirculating air carry out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 520 ℃ of insulation 10h behind 350 ℃ of insulation 5h;
Ingot blank after the homogenizing is carried out surperficial turning, car is added good ingot blank put into process furnace and be heated to 380 ℃ of insulation 5h and put into indirect extrusion machine and push, the container temperature is 350 ℃, and extrusion ratio is 20: 1, and extrusion speed is 2m/min.The bar that extruding is obtained carries out the two-stage time effect processing, and its process system is: be warming up to 200 ℃ of insulation 35h behind 150 ℃ of insulation 5h, air cooling.Bar to above-mentioned preparation is processed into the standard tensile sample according to national standard, carries out room temperature tensile at the Instron8032 drawing machine, and draw speed is 2mm/min.
Present embodiment obtains alloy room temperature tensile performance: tensile strength is 430MPa, and yield strength is 375MPa, and unit elongation is 9%.
Embodiment 2:
The composition of alloy (mass percent) is: Cd content is that 15.0%, Bi content is that 3.0%, Zn content is 5.0%, Y content is that 11.0%, Zr content is that 0.6%, Nb content is 0.5%, the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg.In the present embodiment in the alloy melting process used insulating covering agent each component and weight part thereof be 7.5 gram sulphur, 450 gram diatomite, 247 gram boric acid, silicon sol 45 grams, insulating covering agent accounts for 1.5% of alloy melt gross weight; Refining agent each component and mass percent thereof are 500 gram CaCl
2, 1250 the gram KCl, 125 the gram CaF
2, 625 the gram BaCl
2Mixture, refining agent accounts for 5.0% of alloy melt gross weight.
Weigh up the corresponding ingot metal of total amount 50Kg and master alloy by mentioned component, and load weighted ingot metal and master alloy are put into temperature is that 150 ℃ of baking ovens carry out the preheating of 2h;
Earlier to put into preheating temperature be that 730 ℃ smelting furnace melts for Mg ingot that preheating is good and Mg-25 (or 50) %Y master alloy, need to feed shielding gas and insulating covering agent in the melting process, after treating the above-mentioned raw materials fusing, adopt agitator that alloy liquid is stirred 10min, remove the slag on alloy liquid surface and spread insulating covering agent protected in its surface;
Melt temperature in the smelting furnace is risen to 740 ℃, add metal Bi, master alloy stirs after melting fully, adds Mg-Zr and Zn-Nb master alloy in batches after alloy liquid further is warming up to 790 ℃, and fully stirs; The alloy liquid temp is down to 720 ℃ adds pure Cd and pure Zn, after treating that pure Cd and pure Zn melt fully, adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 50min 700 ℃ of insulations and carry out the cunning semicontinuous casting of low frequency electromagnetic, in castingprocesses, protected with shielding gas; The casting technique system is: electromagnetic field frequency is 30Hz, and magneticstrength is 25mT, and casting speed is 70mm/min, and cooling water inflow is 90L/min, and crystallizer is wrought aluminium cover crystallizer, obtains the ingot blank that diameter is 172mm;
The ingot blank of preparation is put into the resistance-type process furnace that has recirculating air carry out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 510 ℃ of insulation 12h behind 350 ℃ of insulation 8h;
Ingot blank after the homogenizing is carried out surperficial turning, car is added good ingot blank put into process furnace and be heated to 340 ℃ of insulation 8h and put into indirect extrusion machine and push, the container temperature is 320 ℃, and extrusion ratio is 40: 1, and extrusion speed is 1m/min.The bar that extruding is obtained carries out the two-stage time effect processing, and its process system is: be warming up to 200 ℃ of insulation 30h behind 120 ℃ of insulation 6h, air cooling.Bar to above-mentioned preparation is processed into the standard tensile sample according to national standard, carries out room temperature tensile at the Instron8032 drawing machine, and draw speed is 2mm/min.
Present embodiment obtains alloy room temperature tensile performance: tensile strength is 410MPa, and yield strength is 350MPa, and unit elongation is 8%.
Embodiment 3:
The composition of alloy (mass percent) is: Cd content is that 1.0%, Bi content is that 2.0%, Zn content is 7.0%, Y content is that 15.0%, Zr content is that 0.8%, Nb content is 1.2%, the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg.In the present embodiment in the alloy melting process used insulating covering agent each component and weight part thereof be 4 gram sulphur, 225 gram diatomite, 200 gram boric acid, silicon sol 71 grams, insulating covering agent accounts for 1.0% of alloy melt gross weight; Refining agent each component and mass percent thereof are 750 gram CaCl
2, 1350 the gram KCl, 150 the gram CaF
2, 750 the gram BaCl
2Mixture, refining agent accounts for 6.0% of alloy melt gross weight.
Weigh up the corresponding ingot metal of total amount 50Kg and master alloy by mentioned component, and load weighted ingot metal and master alloy are put into temperature is that 200 ℃ of baking ovens carry out the preheating of 3h;
Earlier to put into preheating temperature be that 750 ℃ smelting furnace melts for Mg ingot that preheating is good and Mg-25 (or 50) %Y master alloy, need to feed shielding gas and insulating covering agent in the melting process, after treating the above-mentioned raw materials fusing, adopt agitator that alloy liquid is stirred 10min, remove the slag on alloy liquid surface and spread insulating covering agent protected in its surface;
Melt temperature in the smelting furnace is risen to 720 ℃, add metal Bi, master alloy stirs after melting fully, adds Mg-Zr and Zn-Nb master alloy in batches after alloy liquid further is warming up to 800 ℃, and fully stirs; The alloy liquid temp is down to 720 ℃ adds pure Cd and pure Zn, after treating that pure Cd and pure Zn melt fully, adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 50min 700 ℃ of insulations and carry out the cunning semicontinuous casting of low frequency electromagnetic, in castingprocesses, protected with shielding gas; The casting technique system is: electromagnetic field frequency is 20Hz, and magneticstrength is 30mT, and casting speed is 60mm/min, and cooling water inflow is 70L/min, and crystallizer is wrought aluminium cover crystallizer, obtains the ingot blank that diameter is 200mm;
The ingot blank of preparation is put into the resistance-type process furnace that has recirculating air carry out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 530 ℃ of insulation 15h behind 380 ℃ of insulation 6h;
Ingot blank after the homogenizing is carried out surperficial turning, car is added good ingot blank put into process furnace and be heated to 400 ℃ of insulation 10h and put into indirect extrusion machine and push, the container temperature is 380 ℃, and extrusion ratio is 50: 1, and extrusion speed is 1.5m/min.The bar that extruding is obtained carries out the two-stage time effect processing, and its process system is: be warming up to 220 ℃ of insulation 30h behind 160 ℃ of insulation 3h, air cooling.Bar to above-mentioned preparation is processed into the standard tensile sample according to national standard, carries out room temperature tensile at the Instron8032 drawing machine, and draw speed is 2mm/min.
Alloy that present embodiment obtains records the gained alloy through the X diffraction experiment and belongs to hexagonal system, and unit cell parameters is a=311.87pm, b=310.65pm, c=506.81pm, α=90 °, β=90 °, γ=120 °.
Present embodiment obtains alloy room temperature tensile performance: tensile strength is 450MPa, and yield strength is 380MPa, and unit elongation is 10%.
Embodiment 4:
The composition of alloy (mass percent) is: Cd content is that 1.0%, Bi content is that 10.0%, Zn content is 13.0%, Y content is that 7.0%, Zr content is that 1.0%, Nb content is 2.0%, the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg.In the present embodiment in the alloy melting process used insulating covering agent each component and weight part thereof be 7.5 gram sulphur, 450 gram diatomite, 225 gram boric acid, aluminum phosphate 67.5 grams, insulating covering agent accounts for 1.5% of alloy melt gross weight; Refining agent each component and mass percent thereof are 750 gram CaCl
2, 1000 the gram KCl, 125 the gram CaF
2, 625 the gram BaCl
2Mixture, refining agent accounts for 5.0% of alloy melt gross weight.
Weigh up the corresponding ingot metal of total amount 50Kg and master alloy by mentioned component, and load weighted ingot metal and master alloy are put into temperature is that 180 ℃ of baking ovens carry out the preheating of 2.5h;
Earlier to put into preheating temperature be that 750 ℃ smelting furnace melts for Mg ingot that preheating is good and Mg-25 (or 50) %Y master alloy, need to feed shielding gas and insulating covering agent in the melting process, after treating the above-mentioned raw materials fusing, adopt agitator that alloy liquid is stirred 8min, remove the slag on alloy liquid surface and spread insulating covering agent protected in its surface;
Melt temperature in the smelting furnace is risen to 750 ℃, add metal Bi, master alloy stirs after melting fully, adds Mg-Zr and Zn-Nb master alloy in batches after alloy liquid further is warming up to 780 ℃, and fully stirs; The alloy liquid temp is down to 730 ℃ adds pure Cd and pure Zn, after treating that pure Cd and pure Zn melt fully, adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 60min 710 ℃ of insulations and carry out the cunning semicontinuous casting of low frequency electromagnetic, in castingprocesses, protected with shielding gas; The casting technique system is: electromagnetic field frequency is 25Hz, and magneticstrength is 22mT, and casting speed is 70mm/min, and cooling water inflow is 50L/min, and crystallizer is wrought aluminium cover crystallizer, obtains the ingot blank that diameter is 165mm;
The ingot blank of preparation is put into the resistance-type process furnace that has recirculating air carry out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 520 ℃ of insulation 15h behind 400 ℃ of insulation 5h;
Ingot blank after the homogenizing is carried out surperficial turning, car is added good ingot blank put into process furnace and be heated to 420 ℃ of insulation 8h and put into indirect extrusion machine and push, the container temperature is 400 ℃, and extrusion ratio is 20: 1, and extrusion speed is 5m/min.The bar that extruding is obtained carries out the two-stage time effect processing, and its process system is: be warming up to 200 ℃ of insulation 80h behind 120 ℃ of insulation 8h, air cooling.Bar to above-mentioned preparation is processed into the standard tensile sample according to national standard, carries out room temperature tensile at the Instron8032 drawing machine, and draw speed is 2mm/min.
Alloy that present embodiment obtains records the gained alloy through the X diffraction experiment and belongs to hexagonal system, and unit cell parameters is a=325.26pm, b=326.23pm, c=486.61pm, α=90 °, β=90 °, γ=120 °.
Present embodiment obtains alloy room temperature tensile performance: tensile strength is 450MPa, and yield strength is 373MPa, and unit elongation is 9%.
Embodiment 5:
The composition of alloy (mass percent) is: Cd content is that 4.0%, Bi content is that 3.0%, Zn content is 7.0%, Y content is that 11.0%, Zr content is that 0.4%, Nb content is 0.3%, the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg.In the present embodiment in the alloy melting process used insulating covering agent each component and weight part thereof be 14 gram sulphur, 840 gram diatomite, 420 gram boric acid, silicon sol 126 grams, insulating covering agent accounts for 2.0% of alloy melt gross weight; Refining agent each component and mass percent thereof are 1400 gram CaCl
2, 2520 the gram KCl, 280 the gram CaF
2, 1400 the gram BaCl
2Mixture, refining agent accounts for 8.0% of alloy melt gross weight.
Weigh up the corresponding ingot metal of total amount 70Kg and master alloy by mentioned component, and load weighted ingot metal and master alloy are put into temperature is that 150 ℃ of baking ovens carry out the preheating of 3h;
Earlier to put into preheating temperature be that 740 ℃ smelting furnace melts for Mg ingot that preheating is good and Mg-25 (or 50) %Y master alloy, need to feed shielding gas and insulating covering agent in the melting process, after treating the above-mentioned raw materials fusing, adopt agitator that alloy liquid is stirred 8min, remove the slag on alloy liquid surface and spread insulating covering agent protected in its surface;
Melt temperature in the smelting furnace is risen to 720 ℃, add metal Bi, master alloy stirs after melting fully, adds Mg-Zr and Zn-Nb master alloy in batches after alloy liquid further is warming up to 780 ℃, and fully stirs; The alloy liquid temp is down to 720 ℃ adds pure Cd and pure Zn, after treating that pure Cd and pure Zn melt fully, adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 30min 720 ℃ of insulations and carry out the cunning semicontinuous casting of low frequency electromagnetic, in castingprocesses, protected with shielding gas; The casting technique system is: electromagnetic field frequency is 30Hz, and magneticstrength is 20mT, and casting speed is 40mm/min, and cooling water inflow is 200L/min, and crystallizer is wrought aluminium cover crystallizer, obtains the ingot blank that diameter is 300mm;
The ingot blank of preparation is put into the resistance-type process furnace that has recirculating air carry out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 500 ℃ of insulation 15h behind 300 ℃ of insulation 8h;
Ingot blank after the homogenizing is carried out surperficial turning, car is added good ingot blank put into process furnace and be heated to 420 ℃ of insulation 8h and put into indirect extrusion machine and push, the container temperature is 400 ℃, and extrusion ratio is 20: 1, and extrusion speed is 3m/min.The bar that extruding is obtained carries out the two-stage time effect processing, and its process system is: be warming up to 200 ℃ of insulation 80h behind 120 ℃ of insulation 8h, air cooling.Bar to above-mentioned preparation is processed into the standard tensile sample according to national standard, carries out room temperature tensile at the Instron8032 drawing machine, and draw speed is 2mm/min.
Present embodiment obtains alloy room temperature tensile performance: tensile strength is 425MPa, and yield strength is 365MPa, and unit elongation is 7%.
Embodiment 6:
The composition of alloy (mass percent) is: Cd content is that 7.0%, Bi content is that 8.0%, Zn content is 10.0%, Y content is that 13.0%, Zr content is that 0.5%, Nb content is 0.6%, the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg.In the present embodiment in the alloy melting process used insulating covering agent each component and weight part thereof be 45 gram sulphur, 1650 diatomite, 750 gram boric acid, silicon sol 255 grams, insulating covering agent accounts for 2.0% of alloy melt gross weight; Refining agent each component and mass percent thereof are 2835 gram CaCl
2, 5250 the gram KCl, 315 the gram CaF
2, 2100 the gram BaCl
2Mixture, refining agent accounts for 7.0% of alloy melt gross weight.
Weigh up the corresponding ingot metal of total amount 150Kg and master alloy by mentioned component, and load weighted ingot metal and master alloy are put into temperature is that 180 ℃ of baking ovens carry out the preheating of 2h;
Earlier to put into preheating temperature be that 680 ℃ smelting furnace melts for Mg ingot that preheating is good and Mg-25 (or 50) %Y master alloy, need to feed shielding gas and insulating covering agent in the melting process, after treating the above-mentioned raw materials fusing, adopt agitator that alloy liquid is stirred 10min, remove the slag on alloy liquid surface and spread insulating covering agent protected in its surface;
Melt temperature in the smelting furnace is risen to 750 ℃, add metal Bi, master alloy stirs after melting fully, adds Mg-Zr and Zn-Nb master alloy in batches after alloy liquid further is warming up to 800 ℃, and fully stirs; The alloy liquid temp is down to 740 ℃ adds pure Cd and pure Zn, after treating that pure Cd and pure Zn melt fully, adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 60min 700 ℃ of insulations and carry out the cunning semicontinuous casting of low frequency electromagnetic, in castingprocesses, protected with shielding gas; The casting technique system is: electromagnetic field frequency is 15Hz, and magneticstrength is 30mT, and casting speed is 20mm/min, and cooling water inflow is 400L/min, and crystallizer is wrought aluminium cover crystallizer, obtains the ingot blank that diameter is 400mm;
The ingot blank of preparation is put into the resistance-type process furnace that has recirculating air carry out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 520 ℃ of insulation 15h behind 350 ℃ of insulation 6h;
Ingot blank after the homogenizing is carried out surperficial turning, car is added good ingot blank put into process furnace and be heated to 420 ℃ of insulation 10h and put into indirect extrusion machine and push, the container temperature is 400 ℃, and extrusion ratio is 50: 1, and extrusion speed is 1m/min.The bar that extruding is obtained carries out the two-stage time effect processing, and its process system is: be warming up to 220 ℃ of insulation 50h behind 160 ℃ of insulation 3h, air cooling.Bar to above-mentioned preparation is processed into the standard tensile sample according to national standard, carries out room temperature tensile at the Instron8032 drawing machine, and draw speed is 2mm/min.
Present embodiment obtains alloy room temperature tensile performance: tensile strength is 443MPa, and yield strength is 380MPa, and unit elongation is 8%.
Comparing embodiment 1:
The composition of alloy (mass percent) is: Zn content is that 5.0%, Y content is that 7.0%, Zr content is 0.6%, and the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg.In the present embodiment in the alloy melting process used insulating covering agent each component and weight part thereof be 7.5 gram sulphur, 675 gram diatomite, 600 gram boric acid, silicon sol 217.5 grams, insulating covering agent accounts for 1.0% of alloy melt gross weight; Refining agent each component and mass percent thereof are 1800 gram CaCl
2, 2760 the gram KCl, 240 the gram CaF
2, 1200 the gram BaCl
2Mixture, refining agent accounts for 4.0% of alloy melt gross weight.
Weigh up the corresponding ingot metal of total amount 150Kg and master alloy by mentioned component, and load weighted ingot metal and master alloy are put into temperature is that 180 ℃ of baking ovens carry out the preheating of 2h.Earlier to put into preheating temperature be that 680 ℃ smelting furnace melts for Mg ingot that preheating is good and Mg-25 (or 50) %Y master alloy, after treating the above-mentioned raw materials fusing, adopt agitator that alloy liquid is stirred 10min, remove the slag on alloy liquid surface and spread insulating covering agent protected in its surface; Add Mg-Zr in batches after alloy liquid further is warming up to 800 ℃ and fully stir; Adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 60min 720 ℃ of insulations and carry out the cunning semicontinuous casting of low frequency electromagnetic, in castingprocesses, protected with shielding gas; The casting technique system is: electromagnetic field frequency is 15Hz, and magneticstrength is 30mT, and casting speed is 20mm/min, and cooling water inflow is 400L/min, and crystallizer is wrought aluminium cover crystallizer, obtains the ingot blank that diameter is 400mm.The ingot blank of preparation is put into the resistance-type process furnace that has recirculating air carry out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 520 ℃ of insulation 15h behind 350 ℃ of insulation 6h; Ingot blank after the homogenizing is carried out surperficial turning, car is added good ingot blank put into process furnace and be heated to 420 ℃ of insulation 10h and put into indirect extrusion machine and push, the container temperature is 400 ℃, and extrusion ratio is 50: 1, and extrusion speed is 1m/min.The bar that extruding is obtained carries out the two-stage time effect processing, and its process system is: be warming up to 220 ℃ of insulation 30h behind 150 ℃ of insulation 3h, air cooling.Bar to above-mentioned preparation is processed into the standard tensile sample according to national standard, carries out room temperature tensile at the Instron8032 drawing machine, and draw speed is 2mm/min.
Present embodiment obtains alloy room temperature tensile performance: tensile strength is 323MPa, and yield strength is 220MPa, and unit elongation is 13%.
Comparing embodiment 2:
The composition of alloy (mass percent) is: Zn content is that 7.0%, Y content is that 10.0%, Zr content is that the total amount of 0.6% impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg.In the present embodiment in the alloy melting process used insulating covering agent each component and weight part thereof be 10 gram sulphur, 600 gram diatomite, 300 gram boric acid, aluminum phosphate 90 grams, insulating covering agent accounts for 2.0% of alloy melt gross weight; Refining agent each component and mass percent thereof are 750 gram CaCl
2, 1350 the gram KCl, 150 the gram CaF
2, 750 the gram BaCl
2Mixture, refining agent accounts for 6.0% of alloy melt gross weight.
Weigh up the corresponding ingot metal of total amount 50Kg and master alloy by mentioned component, and load weighted ingot metal and master alloy are put into temperature is that 200 ℃ of baking ovens carry out the preheating of 2h.Earlier to put into preheating temperature be that 700 ℃ smelting furnace melts for Mg ingot that preheating is good and Mg-25 (or 50) %Y master alloy, after treating the above-mentioned raw materials fusing, adopt agitator that alloy liquid is stirred 10min, remove the slag on alloy liquid surface and spread insulating covering agent protected in its surface; Add Mg-Zr in batches after alloy liquid further is warming up to 780 ℃ and fully stir; Adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 50min 740 ℃ of insulations and carry out the cunning semicontinuous casting of low frequency electromagnetic, in castingprocesses, protected with shielding gas; The casting technique system is: electromagnetic field frequency is 20Hz, and magneticstrength is 28mT, and casting speed is 60mm/min, and cooling water inflow is 70L/min, and crystallizer is wrought aluminium cover crystallizer, obtains the ingot blank that diameter is 172mm.The ingot blank of preparation is put into the resistance-type process furnace that has recirculating air carry out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 510 ℃ of insulation 12h behind 350 ℃ of insulation 5h; Ingot blank after the homogenizing is carried out surperficial turning, car is added good ingot blank put into process furnace and be heated to 430 ℃ of insulation 8h and put into indirect extrusion machine and push, the container temperature is 400 ℃, and extrusion ratio is 30: 1, and extrusion speed is 3m/min.The bar that extruding is obtained carries out the two-stage time effect processing, and its process system is: be warming up to 220 ℃ of insulation 30h behind 160 ℃ of insulation 3h, air cooling.Bar to above-mentioned preparation is processed into the standard tensile sample according to national standard, carries out room temperature tensile at the Instron8032 drawing machine, and draw speed is 1mm/min.
Present embodiment obtains alloy room temperature tensile performance: tensile strength is 358MPa, and yield strength is 263MPa, and unit elongation is 6.0%.
Performance compares:
| ? | Tensile strength (MPa) | Yield strength (MPa) | Unit elongation (%) |
| Embodiment 1 | 430 | 375 | 9 |
| Embodiment 2 | 410 | 350 | 8 |
| Embodiment 3 | 450 | 380 | 10 |
| Embodiment 4 | 450 | 373 | 9 |
| Embodiment 5 | 425 | 365 | 7 |
| Embodiment 6 | 443 | 380 | 8 |
| Comparing embodiment 1 | 323 | 220 | 13 |
| Comparing embodiment 2 | 358 | 263 | 6 |
As can be seen from the above table, the application's Mg-Zn-Y-Zr alloy has added after Cd, Bi and the Nb, no matter in tensile strength, still all has significant advantage aspect yield strength, and it has excellent unit elongation simultaneously.
Claims (7)
1. high-strength magnesium alloy, it is characterized in that in the alloy that each component and mass percent thereof are: 1.0～15.0% Cd, 2.0～10.0% Bi, 5.0%～13.0% Zn, 7.0%～15.0% Y, 0.4～1.0% Zr, 0.1～5.0% Nb, the total amount of impurity element Si, Fe, Cu and Ni is less than 0.02%, and surplus is Mg.
2. high-strength magnesium alloy according to claim 1, it is characterized in that in the alloy that each component and mass percent thereof are: Cd content is that 1.0%, Bi content is 2.0%, Zn content is that 7.0%, Y content is that 15.0%, Zr content is 0.8%, Nb content is 1.2%, and the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg, and unit cell parameters is a=311.87pm, b=310.65pm, c=506.81pm, α=90 °, β=90 °, γ=120 °.
3. high-strength magnesium alloy according to claim 1, it is characterized in that in the alloy that each component and mass percent thereof are: Cd content is that 1.0%, Bi content is 10.0%, Zn content is that 13.0%, Y content is that 7.0%, Zr content is 1.0%, Nb content is 2.0%, and the total amount of impurity element Si, Fe, Cu and Ni is surplus less than 0.02%, Mg, and unit cell parameters is a=325.26pm, b=326.23pm, c=486.61pm, α=90 °, β=90 °, γ=120 °.
4. the preparation method of the described high-strength magnesium alloy of claim 1 is characterized in that comprising the steps:
(1) Mg, Cd, Bi, Zn, Y, Nb and Zr are pressed the described ingredient composition of claim 1, wherein Mg, Cd, Bi and Zn add with the form of technical pure Mg, pure Cd, pure Bi, pure Zn, and Y, Nb and Zr add with the form of Mg-25 (or 50) wt.%Y, Zn-30%Nb and Mg-30wt.%Zr master alloy respectively;
(2) place baking oven to carry out preheating respectively described raw material, preheating temperature is 150～200 ℃, and be 2～3h warm up time;
(3) smelting furnace is warming up to 650～750 ℃, the pure Mg of preheating and Mg-Y master alloy are put into smelting furnace to be melted, need feeding shielding gas and insulating covering agent to be protected in the melting process, after treating that above-mentioned raw materials all melts, adopt agitator that alloy liquid is stirred 5～10min and make its even mixing, remove the slag on alloy liquid surface then;
(4) above-mentioned alloy liquid is warming up to 720～750 ℃ and adds metal Bi, master alloy stirs after melting fully, adds Mg-Zr and Zn-Nb master alloy in batches after alloy liquid further is warming up to 780～800 ℃, and fully stirs; The alloy liquid temp is down to 720～740 ℃ adds pure Cd and pure Zn, treat that pure Cd and pure Zn melt fully after; Adopt Ar gas and solvent that alloy liquid is carried out refining treatment, melt through stir and skim after leave standstill 30～60min 700～720 ℃ of insulations and cast;
(5) ingot blank of casting in the step (4) is put into the resistance-type process furnace that has recirculating air and carry out the processing of twin-stage homogenizing, homogenizing processing system is: be warming up to 500～530 ℃ of insulation 10～15h behind 350～400 ℃ of insulation 5～8h;
(6) ingot blank after the homogenizing in the step (5) is carried out surperficial turning, ingot blank diameter and length are worked into extrusion machine internal diameter of the container and length are complementary; The ingot blank that processes is put into process furnace be heated to 340～420 ℃, insulation 5～10h;
(7) container that the ingot blank that heats in the step (6) is put into prior preheating pushes, and extrusion speed is 1.0～5.0m/min, and the container preheating temperature is 320～400 ℃, and extrusion ratio is 10～50: 1, obtains extruded bars;
(8) extruded bars that step (7) is obtained carries out the two-stage time effect processing, and its process system is: be warming up to 180～220 ℃ of insulation 30～80h behind 120～160 ℃ of insulation 3～8h, air cooling makes the high-strength magnesium alloy material.
5. preparation method according to claim 4, it is characterized in that the cunning semi-continuous casting method of casting employing low frequency electromagnetic in the described step (4), the casting technique system is: electromagnetic field frequency is 15～30Hz, magneticstrength is 15～30mT, casting speed is 20～80mm/min, cooling water inflow is 50～400L/min, and crystallizer is wrought aluminium cover crystallizer.
6. preparation method according to claim 4 is characterized in that described shielding gas is SF
6+ CO
2+ Ar mixed gas, SF
6: CO
2: the Ar volume ratio is 0.5: 40: 50.
7. preparation method according to claim 4, it is characterized in that the magnesium alloy mechanical property index of described preparation is as follows: tensile strength is 410～450MPa, and yield strength is 350～380MPa, and unit elongation is greater than 6%.
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