CN115652158A - Creep-resistant Mg-Al wrought magnesium alloy and preparation method thereof - Google Patents
Creep-resistant Mg-Al wrought magnesium alloy and preparation method thereof Download PDFInfo
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Abstract
A creep-resistant Mg-Al wrought magnesium alloy and a preparation method thereof comprise the following components in percentage by weight: 7 to 9 percent of Al, 0.2 to 0.5 percent of Zn, 0 to 0.5 percent of Y, 0 to 0.4 percent of Ca, 0 to 0.5 percent of Nd, and the balance of Mg. The method adopts the design of multiple microalloying components, selects reasonable microalloying elements or combinations, and obtains the variable-form Mg-Al alloy with stronger basal plane texture and uniform and refined tissue through the processes of cleaning smelting and ingot casting, homogenization treatment, extrusion forming and annealing treatment, and the variable-form Mg-Al alloy has higher tensile strength and elongation at break; secondly, the multi-element microalloying effectively inhibits the grain boundary migration caused by the dynamic discontinuous precipitation of the grain boundary in the medium-temperature creep process, enhances the stability of the grain boundary, and reduces the sensitivity of the discontinuous precipitation to stress in the creep process; meanwhile, the multielement microalloying promotes the fine and continuous precipitation in the crystal, and enhances the pinning effect on the movement of dislocation in the crystal. The comprehensive effect realizes the preparation of the high-performance Mg-Al wrought magnesium alloy with low cost and higher mechanical property and medium-temperature creep resistance.
Description
Technical Field
The invention belongs to the technical field of creep-resistant wrought magnesium alloy, and particularly relates to a creep-resistant Mg-Al wrought magnesium alloy and a preparation method thereof.
Background
Magnesium-aluminum (Mg-Al) series magnesium alloy is the most widely commercially used industrial magnesium alloy, and the heat-treatable Mg-Al alloy represented by AZ80 (Mg-8 Al-0.5Zn-0.2Mn, wt.%) has good casting performance, mechanical strength (extrusion yield strength is 200-280 MPa) and considerable plasticity (elongation at break is more than 10%), and has obvious application advantages in various fields such as communication, traffic, medical treatment and the like. With the increasing service requirements of magnesium alloy in the medium-temperature environment, such as magnesium alloy airplane hubs, automobile engine parts, microwave probe station micro-chambers and the like, the magnesium alloy is required to have better medium-temperature creep resistance.
The prior creep-resistant magnesium alloy adopts single or multiple rare earth elements which are mainly alloy elements, and the creep-resistant magnesium alloy is limited in large-scale application due to high raw material cost, low yield in the casting process, complex casting process, low final ingot casting or casting yield and high comprehensive cost. The high volume content of the rare earth thermally stable phase is liable to induce brittleness, resulting in higher strength but generally poorer plasticity.
Disclosure of Invention
The invention aims to provide a creep-resistant Mg-Al wrought magnesium alloy and a preparation method thereof, aiming at solving the problems that the creep-resistant magnesium alloy is limited in scale application due to high raw material cost, low yield in the casting process, complex casting process, low final ingot or casting yield and high comprehensive cost. The high volume content rare earth thermal stable phase is easy to induce brittleness, so that the strength is higher but the plasticity is generally poorer.
In order to achieve the purpose, the invention adopts the following technical scheme:
a creep-resistant Mg-Al wrought magnesium alloy comprises the following components in percentage by weight: 7 to 9 percent of Al, 0.2 to 0.5 percent of Zn, 0 to 0.5 percent of Y, 0 to 0.4 percent of Ca, 0 to 0.5 percent of Nd, and the balance of Mg.
Further, the preparation method of the creep-resistant Mg-Al wrought magnesium alloy comprises the following steps:
preparing alloy raw materials and auxiliary materials by adopting a purified magnesium alloy semi-continuous casting system;
gradually adjusting the temperature of a purified magnesium alloy semi-continuous casting system according to a smelting process, adding material adjusting components, then sequentially carrying out high-temperature gradient standing for impurity removal, carrying out secondary adjustment on infinitesimal components, and then carrying out casting and forming;
and carrying out plastic forming treatment on the cast and formed product to obtain the creep-resistant multi-microalloyed Mg-Al deformation alloy.
Furthermore, in the purified magnesium alloy semi-continuous casting system, the crucible is a graphite crucible, and the volume density of the graphite crucible is 1.82-1.85g/cm 3 The heat conductivity is 85W/m.K, the ash content is 500ppm, the purified ash content is 11ppm, and the granularity is 8-11 mu m; the catheter adopts a 304 stainless steel pipe; the crystallizer adopts the graphite inner wall; the cooling medium is industrial water.
Further, the purity of the alloy raw materials and auxiliary materials is as follows: 99.98% magnesium, 99.994% aluminum, 99.995% zinc; the microalloy elements are added in a master alloy form: 99.9% Mg-30Y, 99.9% Mg-20Ca, 99.9% Mg-30Nd; the flux adopts No. 5 flux: mgCl 2 =46-54%, KCl =29-33%, naCl =17-21%, water-insoluble matter ≤ 1.5%, water content ≤ 1%; the shielding gas was 99.999% argon.
Further, the smelting process gradually adjusts the temperature and timely adds the material adjusting components:
a) Heating up in steps for protection for standby: heating a completely-debugged purified magnesium alloy semi-continuous casting system to 300 ℃ and preserving heat for 2h, introducing argon into an exposed area of a graphite crucible to protect and continuously heating to 600 ℃ and preserving heat for 1h, and then heating to 750 ℃ for later use;
b) Detecting a main element alloy molten material: firstly, casting ingots of magnesium, zinc and aluminum into a crucible according to the alloy proportioning components and the burning loss rate of alloy elements; keeping the temperature at 740-750 ℃ to ensure that all the input materials are melted, stirring the materials in the solution for about 10-15 minutes by adopting argon, and taking a melt sample to perform primary stokehole component detection;
c) Detecting primary refining components: refining the No. 5 flux with the total melt mass of 1-3% at 740-750 ℃ for 10-15 minutes, stirring the refined flux in the solution by adopting argon, and taking a melt sample to perform secondary stokehole component detection;
d) Adjusting the components of the micro-element alloy: adding magnesium, zinc, aluminum and Mg-30Y, mg-30Nd cast ingots, adjusting alloy components, then carrying out secondary refining, refining at 740-750 ℃ by using No. 5 flux with the total melt mass of about 1-3% by mass, and stirring in the solution for about 10-15 minutes by adopting argon; and taking a melt sample for carrying out third stokehole component detection to ensure that the components of the micro-element alloy are within a set range.
Further, high-temperature echelon standing for impurity removal: keeping the temperature of the magnesium liquid at 750 ℃ and standing for 15-20 minutes, then removing slag at the bottom of the crucible, and keeping the temperature of the magnesium liquid at 720-730 ℃ and standing for 10-15 minutes; taking a melt sample for fourth stokehole component detection to ensure that the components of the micro-element alloy are within a set range;
secondary adjustment of the microelement: adding Mg-20Ca cast ingot at the melt temperature of 720-730 ℃, stirring in the solution for about 2-5 minutes by adopting argon, adjusting the alloy components to be within a set range, and preparing for casting.
Further, a crystallizer is used for casting and forming: raising the temperature of the melt to 750-760 ℃, closing a furnace cover, and putting the melt into a liquid guide pipe under high-purity argon pressure to start pouring; the temperature of the tundish is kept between 690 and 700 ℃, the ingot pulling speed of the casting machine is kept between 50 and 200mm/min, and the flow rate of cooling water is kept between 3 and 5m 3 And h, peeling the semi-continuous casting rod, carrying out visual detection without loose and shrinkage cavity impurities visible to naked eyes, and cutting the material for later use according to the requirements of a plastic forming process.
Further, plastic forming treatment:
a) Homogenizing: homogenizing the scalped multi-element microalloyed Mg-Al alloy cast ingot in a protective atmosphere at 400-420 ℃ for 20-30h, wherein the cooling mode is water quenching;
b) Plastic forming: performing thermal mechanical treatment on the multi-element microalloyed Mg-Al alloy homogenized cast ingot;
c) Heat treatment after forming: and annealing the multi-element microalloyed Mg-Al wrought magnesium alloy.
Further, the thermo-mechanical treatment is extrusion treatment: temperature of the extrusion die: 350-400 ℃, extrusion working speed: 0.3-1mm/min, setting the temperature of the extrusion cylinder: 300-350 ℃, setting the extrusion ratio: 10-30, and the extrusion discharge is drawn by a tractor, and the traction force is about 100-500N.
Furthermore, the annealing temperature range is 300-420 ℃, and the annealing time is 2-8h.
Compared with the prior art, the invention has the following technical effects:
the method adopts the design of multiple microalloying components, selects reasonable microalloying elements or combinations, and obtains the variable-form Mg-Al alloy with stronger basal plane texture and uniform and refined tissue through the processes of cleaning smelting and ingot casting, homogenization treatment, extrusion forming and annealing treatment, and the variable-form Mg-Al alloy has higher tensile strength and elongation at break; secondly, the multi-element microalloying effectively inhibits the grain boundary migration caused by the dynamic discontinuous precipitation of the grain boundary in the medium-temperature creep process, enhances the stability of the grain boundary, and reduces the sensitivity of the discontinuous precipitation to stress in the creep process; meanwhile, the multielement microalloying promotes the fine and continuous precipitation in the crystal, and enhances the pinning effect on the movement of dislocation in the crystal. The comprehensive effect realizes the preparation of the high-performance Mg-Al wrought magnesium alloy with low cost and higher mechanical property and medium-temperature creep resistance.
The medium-temperature creep resistance of the variable-form Mg-Al alloy is improved by a multi-element microalloying method, the used alloy elements are less, the cost is low, and the processing and forming are easy.
According to the invention, the multi-microalloying is adopted to inhibit the dynamic discontinuous precipitation of the grain boundary in the creep process by acting on the local area of the grain boundary, so that the continuous precipitation in the grain is promoted, the fine homogenization of the grain structure is facilitated, and the tensile strength and the fracture elongation of the morphotropic magnesium alloy are improved.
The invention regulates and controls the organization characteristics before creep and during creep by multi-microalloying, and does not generate adverse effect on the forming size precision. Meanwhile, the fine and uniform grain structure can be promoted, and the tensile strength and the breaking elongation of the section are improved.
According to the invention, by a multi-element microalloying method, fine homogenization distribution (< 100 mu m) of the size of extruded crystal grains is realized, the texture of the basal plane of the plate is strengthened, and the creep resistance of the plate is increased by improving the mechanical strength in the extrusion direction under the combined action of the fine homogenization distribution and the basal plane texture.
Drawings
FIG. 1 is a comparison of steady state creep rate and room temperature tensile strength at 100-150 deg.C/50-100 MPa for cast Mg-Al alloys and the creep resistant extruded Mg-Al alloys of the present invention.
FIG. 2 is a graph showing the results of EBSD analysis.
FIG. 3 is a comparison graph of mechanical strength of a multi-microalloyed Mg-Al alloy AZ 80M.
Figure 4 shows a comparison of basal plane texture strength of multi-microalloyed Mg-Al alloy AZ80M compared with common commercial AZ80 magnesium alloy.
FIG. 5 is a graph showing the gradient change of the DP content of the end gradient stress region and the corresponding Vickers hardness value after the AZ80 magnesium alloy creeps at 125 ℃/50 MPa.
FIG. 6 is a graph showing the variation of the DP content in the gradient stress region of the tip and the corresponding Vickers hardness value after 125 ℃/50MPa creep of the multi-component microalloyed AZ80M magnesium alloy.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
the alloy designed by the invention comprises the following components: the components and the weight percentage thereof are as follows: 7 to 9 percent of Al, 0.2 to 0.5 percent of Zn, 0 to 0.5 percent of Y, 0 to 0.4 percent of Ca, 0 to 0.5 percent of Nd, and the balance of Mg.
The alloy adopts a pure preparation technical scheme, which comprises the following steps
(1) Adopts a semi-continuous casting system of pure magnesium alloy, and the crucible is a high-purity high-density graphite crucible (volume density is 1.82-1.85 g/cm) 3 The thermal conductivity is 85W/(m.K), the ash content is 500ppm, the purified ash content is 11ppm, and the granularity is 8-11 μm); the catheter is made of 304 stainless steel; the crystallizer adopts the graphite inner wall;the cooling medium is industrial water.
(2) The purity of the prepared alloy raw materials and auxiliary materials is controlled, and the purity of magnesium (99.98%), aluminum (99.994%) and zinc (99.995%) are controlled; the microalloy elements are added in a master alloy form: mg-30Y (99.9%), mg-20Ca (99.9%), mg-30Nd (99.9%); the flux is No. 5 flux (MgCl) 2 =46-54%, KCl =29-33%, naCl =17-21%, water-insoluble matter ≤ 1.5%, water content ≤ 1%); the shielding gas was argon (99.999%).
(3) Gradually adjusting the temperature and adding material adjusting components at proper time according to the following smelting process
a) Heating up in steps for protection for standby: heating the well-debugged purified magnesium alloy semi-continuous casting system to 300 ℃ and preserving heat for 2h, introducing argon protection into an exposed area of the graphite crucible, continuously heating to 600 ℃ and preserving heat for 1h, and then heating to 750 ℃ for later use.
b) Detecting a main element alloy molten material: according to the alloy proportioning components and the burning loss rate of alloy elements, firstly, casting ingots of magnesium, zinc and aluminum are put into a crucible, and the casting ingots are lightly placed during feeding, so that the graphite crucible is prevented from being damaged. Keeping the temperature at 740-750 ℃ to ensure that all the input materials are melted, stirring the materials in the solution for about 10-15 minutes by adopting argon, and taking a melt sample to carry out primary stokehole component detection.
c) Detecting primary refining components: refining the No. 5 flux with the mass ratio of 1-3% of the total melt mass at 740-750 ℃ for 10-15 minutes, stirring the refined flux in the solution by adopting argon, and taking a melt sample to perform secondary stokehole component detection.
d) Adjusting the components of the micro-element alloy: adding magnesium, zinc, aluminum and Mg-30Y, mg-30Nd cast ingots, adjusting alloy components, then carrying out secondary refining, refining at 740-750 ℃ by using No. 5 flux with the mass ratio of about 1-3% of the total melt mass, and stirring in the solution for about 10-15 minutes by adopting argon gas. And taking a melt sample for carrying out third stokehole component detection to ensure that the components of the micro-element alloy are within a set range.
e) High-temperature echelon standing for impurity removal: keeping the temperature of the magnesium liquid at 750 ℃ and standing for 15-20 minutes, then removing slag (flux, impurity sediment and the like) at the bottom of the crucible, and keeping the temperature of the magnesium liquid at 720-730 ℃ and standing for 10-15 minutes. And taking a melt sample for fourth stokehole component detection to ensure that the components of the micro-element alloy are within a set range.
f) Secondary adjustment of the microelement: adding Mg-20Ca ingot at the melt temperature of 720-730 ℃, stirring in the solution for about 2-5 minutes by adopting argon, adjusting the alloy components to be within a set range, and preparing for casting.
g) Casting and forming by a crystallizer: the temperature of the melt is raised to 750-760 ℃, the furnace cover is closed, and the high-purity argon pressure of the melt is introduced into the liquid guide pipe to start pouring. The temperature of the tundish is kept between 690 and 700 ℃, the ingot pulling speed of the casting machine is kept between 50 and 200mm/min, and the flow rate of cooling water is kept between 3 and 5m 3 /h。
h) Appearance inspection and material taking: after the semi-continuous casting rod is subjected to skinning treatment, visual detection is carried out to avoid visible looseness, shrinkage cavity, inclusions and the like, and the material is cut according to the requirements of a plastic forming process for later use.
(4) Plastic forming
a) Homogenizing: homogenizing the scalped multi-element microalloyed Mg-Al alloy cast ingot in a protective atmosphere (such as high-purity argon) at 400-420 ℃ for 20-30h, wherein the cooling mode is water quenching.
b) Plastic forming: and performing thermal mechanical treatment on the multi-element microalloyed Mg-Al alloy homogenized ingot by adopting plastic forming methods such as extrusion, forging, rolling and the like. As for extrusion molding, extrusion die temperature: 350-400 ℃, extrusion working speed: 0.3-1mm/min, setting the temperature of the extrusion cylinder: 300-350 ℃, setting the extrusion ratio: 10-30, and the extrusion discharge is drawn by a tractor, and the traction force is about 100-500N.
c) Heat treatment after forming: the multi-element microalloyed Mg-Al wrought magnesium alloy is annealed at the temperature of 300-420 ℃ for 2-8h.
Thus, the preparation of the creep-resistant multi-microalloyed Mg-Al wrought alloy is completed.
The alloy comprises the following components: mg-8Al-0.5Zn-0.2Y-0.15Ca (wt.%).
Creep-resistant multi-microalloying Mg-Al wrought alloy preparation system
(1) Adopting pure purification smeltingPreparing a system, wherein the crucible is a high-purity high-density graphite crucible (the volume density is 1.82-1.85 g/cm) 3 The thermal conductivity is 85W/(m.K), the ash content is 500ppm, the purified ash content is 11ppm, and the granularity is 8-11 μm); the catheter is made of 304 stainless steel; the crystallizer adopts the graphite inner wall; the cooling medium is industrial water.
(2) The raw materials are magnesium (99.98%), aluminum (99.994%) and zinc (99.995%); y and Ca microalloy elements are added in the form of intermediate alloy of Mg-30Y (99.9%) and Mg-20Ca (99.9%); the flux is No. 5 flux (MgCl) 2 =46-54%, KCl =29-33%, naCl =17-21%, water-insoluble matter ≤ 1.5%, water content ≤ 1%); the shielding gas was argon (99.999%).
Preparation process of creep-resistant multi-element microalloyed Mg-Al wrought alloy
(1) Heating the clean magnesium alloy semi-continuous casting system which is well debugged to 300 ℃ and preserving heat for 2h, introducing argon protection into an exposed area of the graphite crucible, continuously heating to 600 ℃ and preserving heat for 1h, and then heating to 750 ℃ for later use.
(2) According to the proportion components of Mg-8Al-0.5Zn-0.2Y-0.15Ca (wt.%) in the total amount of 50kg and the burn-out rate of alloy elements, firstly, casting ingots of magnesium, zinc and aluminum are put into a crucible, and the casting ingots need to be lightly placed during feeding so as to avoid damaging the graphite crucible. Keeping the temperature at 740-750 ℃ to ensure that all the input materials are melted, stirring the materials in the solution for about 10-15 minutes by adopting argon, and taking a melt sample to carry out primary stokehole component detection.
(3) Refining with 0.5kg of No. 5 flux at 740-750 deg.C for 10-15 min, and taking a melt sample for secondary stokehole component detection after the stirring of argon in the solution is completed.
(4) Adding magnesium, zinc, aluminum and Mg-30Y, adjusting alloy components, then carrying out secondary refining, refining about 0.5kg of No. 5 flux at 740-750 ℃, and stirring in the solution for about 10-15 minutes by adopting argon. And taking a melt sample for carrying out third stokehole component detection to ensure that the components of the micro-element alloy are within a set range.
(5) Keeping the temperature of the magnesium liquid at 750 ℃ and standing for 15-20 minutes, then removing slag (flux, impurity sediment and the like) at the bottom of the crucible, and keeping the temperature of the magnesium liquid at 720-730 ℃ and standing for 10-15 minutes. Therefore, the replacement reaction of the residual solvent NaCl and the subsequently added calcium-containing intermediate alloy can be avoided as much as possible, and the burning loss of Ca and the excessive introduction of Na impurities are caused. And taking a melt sample for fourth stokehole component detection to ensure that the components of the micro-element alloy are within a set range.
(6) Adding Mg-20Ca intermediate alloy ingot at the melt temperature of 720-730 ℃, stirring for about 2-5 minutes in the solution by adopting argon, adjusting the alloy components to be within a set range, and preparing for casting.
(7) The temperature of the melt is raised to 750-760 ℃, the furnace cover is closed, and the melt is pressurized into the liquid guide pipe by high-purity argon gas to start casting in the crystallizer. The temperature of the tundish is kept between 690 and 700 ℃, the ingot pulling speed of the casting machine is kept between 50 and 200mm/min, and the flow rate of cooling water is kept between 3 and 5m 3 /h。
(8) Peeling the cast ingot, visually detecting that no loose or shrinkage inclusion is visible to naked eyes, and turning the cast ingot to cut the cast ingot into a bar material with the diameter of 65mm multiplied by 150mm for later use according to an extrusion forming process.
(9) Homogenizing the prepared phi 65mm multiplied by 150mm multi-element microalloyed Mg-Al alloy bar under the protection of argon, wherein the homogenizing parameter is 400 ℃, and water quenching is carried out at room temperature for 24 hours.
(10) Adopting a 300T horizontal extruder to extrude and form the homogenized bar material with the diameter of 65mm multiplied by 150mm, wherein the extruded section material is a plate material with the section size of 55 multiplied by 3.5mm, and the temperature of an extrusion die is as follows: 400 ℃, extrusion working speed: 0.3mm/min, extruder barrel temperature setting: 320 ℃, setting of extrusion ratio: 17, adopting a traction machine to draw the extruded material, wherein the traction force is about 200N.
(11) And annealing the multi-component microalloyed Mg-8Al-0.5Zn-0.2Y-0.15Ca (wt.%) wrought magnesium alloy at the temperature of 420 ℃ for 4h and 7h.
Creep-resistant multi-microalloying Mg-Al deformation alloy performance test
And (3) performing creep property test on the multi-element microalloyed Mg-8Al-0.5Zn-0.2Y-0.15Ca (wt.%) annealed sheet by adopting a uniaxial tensile creep test method, and performing room temperature mechanical property test on the sheet by adopting a room temperature uniaxial tensile mechanical property test method. The test results are shown in table 1. Therefore, the method realizes the high-performance Mg-Al wrought magnesium alloy with high mechanical property and medium-temperature creep resistance at low cost.
TABLE 1 creep-resistant multicomponent microalloyed Mg-Al wrought alloy example 1 mechanical Properties and creep Properties
Example II
The design alloy comprises the following components: mg-8Al-0.5Zn-0.1Y-0.Nd (wt.%).
Creep-resistant multi-microalloying Mg-Al wrought alloy preparation system
(1) Adopts a pure smelting preparation system, and the crucible is a high-purity high-density graphite crucible (volume density is 1.82-1.85 g/cm) 3 The thermal conductivity is 85W/(m.K), the ash content is 500ppm, the purified ash content is 11ppm, and the granularity is 8-11 μm); the catheter is made of 304 stainless steel; the crystallizer adopts the graphite inner wall; the cooling medium is industrial water.
(2) The raw materials are magnesium (99.98%), aluminum (99.994%) and zinc (99.995%); y and Nd microalloy elements are added in the form of Mg-30Y (99.9%) and Mg-30Nd (99.9%) master alloy; the flux is No. 5 flux (MgCl) 2 =46-54%, KCl =29-33%, naCl =17-21%, water-insoluble matter ≤ 1.5%, water content ≤ 1%); the shielding gas was argon (99.999%).
Preparation process of creep-resistant multi-element microalloyed Mg-Al wrought alloy
(1) Heating the clean magnesium alloy semi-continuous casting system which is well debugged to 300 ℃ and preserving heat for 2h, introducing argon protection into an exposed area of the graphite crucible, continuously heating to 600 ℃ and preserving heat for 1h, and then heating to 750 ℃ for later use.
(2) According to the proportion components of Mg-8Al-0.5Zn-0.1Y-0.1Nd (wt.%) alloy and the burn-out rate of alloy elements in the total amount of 50kg, firstly, casting ingots of magnesium, zinc and aluminum are put into a crucible, and the casting ingots need to be lightly placed during feeding so as to avoid damaging the graphite crucible. Keeping the temperature at 740-750 ℃ to ensure that all the input materials are melted, stirring the materials in the solution for about 10-15 minutes by adopting argon, and taking a melt sample to carry out primary stokehole component detection.
(3) Refining with 0.5kg of No. 5 flux at 740-750 deg.C for 10-15 min, and taking a melt sample for secondary stokehole component detection after the stirring of argon in the solution is completed.
(4) Adding Mg, zn, al, mg-30Y and Mg-30Nd to regulate the components, secondary refining to refine No. 5 flux of 0.5kg at 740-750 deg.c and stirring in argon solution for 10-15 min. And taking a melt sample for carrying out third stokehole component detection to ensure that the components of the micro-element alloy are within a set range.
(5) Keeping the temperature of the magnesium liquid at 750 ℃ and standing for 15-20 minutes, then removing slag (flux, impurity sediment and the like) at the bottom of the crucible, and keeping the temperature of the magnesium liquid at 720-730 ℃ and standing for 10-15 minutes. And taking the melt sample for fourth stokehole component detection to ensure that the components of the micro-element alloy are in a set range.
(6) The temperature of the melt is raised to 750-760 ℃, the furnace cover is closed, and the melt is pressurized into the liquid guide pipe by high-purity argon gas to start casting in the crystallizer. The temperature of the tundish is kept between 690 and 700 ℃, the ingot pulling speed of the casting machine is kept between 50 and 200mm/min, and the flow rate of cooling water is kept between 3 and 5m 3 /h。
(7) Peeling the cast ingot, visually detecting that no loose or shrinkage inclusion is visible to naked eyes, and turning the cast ingot to cut the cast ingot into a bar material with the diameter of 65mm multiplied by 150mm for later use according to an extrusion forming process.
(8) Homogenizing the prepared phi 65mm multiplied by 150mm multi-element microalloyed Mg-Al alloy bar under the protection of argon, wherein the homogenizing parameter is 400 ℃, and water quenching is carried out at room temperature for 24 hours.
(9) Adopting a 300T horizontal extruder to extrude and form the homogenized bar material with the diameter of 65mm multiplied by 150mm, wherein the extruded section material is a plate material with the section size of 55 multiplied by 3.5mm, and the temperature of an extrusion die is as follows: 400 ℃, extrusion working speed: 0.3mm/min, extruder barrel temperature setting: 320 ℃, setting of extrusion ratio: 17, adopting a traction machine to draw the extruded material, wherein the traction force is about 200N.
(10) The multi-element microalloyed Mg-8Al-0.5Zn-0.1Y-0.1Nd (wt.%) wrought magnesium alloy is annealed at the temperature of 420 ℃ for 7 hours.
Creep-resistant multi-microalloying Mg-Al deformation alloy performance test
The creep property test of the multi-microalloyed Mg-8Al-0.5Zn-0.1Y-0.1Nd (wt.%) annealed sheet material was performed by the uniaxial tensile creep test method, and the test results are shown in Table 2.
TABLE 2 creep resistance test results for creep-resistant multicomponent microalloyed Mg-Al wrought alloy example 2
Example three
The design alloy comprises the following components: mg-8Al-0.5Zn-0.2Y (wt.%).
Creep-resistant multi-microalloying Mg-Al wrought alloy preparation system
(1) Adopts a pure smelting preparation system, and the crucible is a high-purity high-density graphite crucible (volume density is 1.82-1.85 g/cm) 3 The thermal conductivity is 85W/(m.K), the ash content is 500ppm, the purified ash content is 11ppm, and the granularity is 8-11 μm); the catheter is made of 304 stainless steel; the crystallizer adopts the graphite inner wall; the cooling medium is industrial water.
(2) The raw materials are magnesium (99.98%), aluminum (99.994%) and zinc (99.995%); y microalloy element is added in the form of Mg-30Y (99.9%) master alloy; the flux is No. 5 flux (MgCl) 2 =46-54%, KCl =29-33%, naCl =17-21%, water-insoluble matter ≤ 1.5%, water content ≤ 1%); the shielding gas was argon (99.999%).
Preparation process of creep-resistant multi-element microalloyed Mg-Al wrought alloy
(1) Heating the clean magnesium alloy semi-continuous casting system which is well debugged to 300 ℃ and preserving heat for 2h, introducing argon protection into an exposed area of the graphite crucible, continuously heating to 600 ℃ and preserving heat for 1h, and then heating to 750 ℃ for later use.
(2) According to the proportion components of Mg-8Al-0.5Zn-0.2Y (wt.%) alloy and the burn-out rate of alloy elements of 50kg total weight, firstly, casting ingots of magnesium, zinc and aluminum are put into a crucible, and the casting ingots need to be lightly placed during feeding, so that the graphite crucible is prevented from being damaged. Keeping the temperature at 740-750 ℃ to ensure that all the input materials are melted, stirring the materials in the solution for about 10-15 minutes by adopting argon, and taking a melt sample to carry out primary stokehole component detection.
(3) Refining with 0.5kg of No. 5 flux at 740-750 deg.C for 10-15 min, and taking a melt sample for secondary stokehole component detection after the stirring of argon in the solution is completed.
(4) Adding magnesium, zinc, aluminum and Mg-30Y to adjust the alloy components, then carrying out secondary refining, refining about 0.5kg of No. 5 flux at 740-750 ℃, and stirring in the solution for about 10-15 minutes by adopting argon. And taking a melt sample for carrying out third stokehole component detection to ensure that the components of the micro-element alloy are within a set range.
(5) Keeping the temperature of the magnesium liquid at 750 ℃ and standing for 15-20 minutes, then removing slag (flux, impurity sediment and the like) at the bottom of the crucible, and keeping the temperature of the magnesium liquid at 720-730 ℃ and standing for 10-15 minutes. And taking the melt sample for fourth stokehole component detection to ensure that the components of the micro-element alloy are in a set range.
(6) The temperature of the melt is raised to 750-760 ℃, the furnace cover is closed, and the melt is pressurized into the liquid guide pipe by high-purity argon gas to start casting in the crystallizer. The temperature of the tundish is kept between 690 and 700 ℃, the ingot pulling speed of the casting machine is kept between 50 and 200mm/min, and the flow rate of cooling water is kept between 3 and 5m 3 /h。
(7) Peeling the cast ingot, visually detecting that no loose or shrinkage inclusion is visible to naked eyes, and turning the cast ingot to cut the cast ingot into a bar material with the diameter of 65mm multiplied by 150mm for later use according to an extrusion forming process.
(8) Homogenizing the prepared phi 65mm multiplied by 150mm multi-element microalloyed Mg-Al alloy bar under the protection of argon, wherein the homogenizing parameter is 400 ℃, and the homogenizing parameter is 24 hours, and the room temperature water quenching is carried out.
(9) Adopting a 300T horizontal extruder to extrude and form the homogenized bar material with the diameter of 65mm multiplied by 150mm, wherein the extruded section material is a plate material with the section size of 55 multiplied by 3.5mm, and the temperature of an extrusion die is as follows: 400 ℃, extrusion working speed: 0.3mm/min, extruder barrel temperature setting: 320 ℃, setting of extrusion ratio: 17, adopting a traction machine to draw the extruded material, wherein the traction force is about 200N.
(10) The multi-element microalloyed Mg-8Al-0.5Zn-0.2Y (wt.%) wrought magnesium alloy is annealed at the temperature of 420 ℃ for 7 hours.
Creep-resistant multi-microalloying Mg-Al deformation alloy performance test
The creep performance of the multi-microalloyed Mg-8Al-0.5Zn-0.2Y (wt.%) as annealed sheet above was tested by the uniaxial tensile creep test method, and the test results are shown in Table 2.
TABLE 3 creep resistance test results for creep-resistant multicomponent microalloyed Mg-Al wrought alloy example 3
Comparative example
The alloy components of the comparative case are as follows: mg-8Al-0.5Zn-0.2Mn (wt.%), i.e. ordinary commercial AZ80 magnesium alloy.
Alloy preparation system
(1) Adopts a pure smelting preparation system, and the crucible is a high-purity high-density graphite crucible (volume density is 1.82-1.85 g/cm) 3 The thermal conductivity is 85W/(m.K), the ash content is 500ppm, the purified ash content is 11ppm, and the granularity is 8-11 μm); the catheter is made of 304 stainless steel; the crystallizer adopts the graphite inner wall; the cooling medium is industrial water.
(2) The raw materials are magnesium (99.98%), aluminum (99.994%), zinc (99.995%) and Mg-5Mn (99.9%); the flux is No. 5 flux (MgCl) 2 =46-54%, KCl =29-33%, naCl =17-21%, water-insoluble matter ≤ 1.5%, water content ≤ 1%); the shielding gas was argon (99.999%).
Comparative example preparation of ordinary Mg-Al wrought alloy
(1) Heating the clean magnesium alloy semi-continuous casting system which is well debugged to 300 ℃ and preserving heat for 2h, introducing argon protection into an exposed area of the graphite crucible, continuously heating to 600 ℃ and preserving heat for 1h, and then heating to 750 ℃ for later use.
(2) According to the proportion components of the Mg-8Al-0.5Zn-0.2Mn (wt.%) alloy and the burn-out rate of alloy elements of 50kg total amount, firstly, casting a magnesium, zinc, aluminum and Mg-5Mn intermediate alloy ingot into a crucible, and lightly placing the ingot during feeding to avoid damaging the graphite crucible. Keeping the temperature at 740-750 ℃ to ensure that all the input materials are melted, stirring the materials in the solution for about 10-15 minutes by adopting argon, and taking a melt sample to carry out primary stokehole component detection.
(3) Refining with 0.5kg of No. 5 flux at 740-750 deg.C for 10-15 min, and taking a melt sample for secondary stokehole component detection after the stirring of argon in the solution is completed.
(4) Adding Mg, zn, al and Mg-Mn gold alloy to regulate alloy components, secondary refining to refine No. 5 flux of 0.5kg at 740-750 deg.c, and stirring in argon solution for 10-15 min. And taking a melt sample for carrying out third stokehole component detection to ensure that the alloy components are in a set range.
(5) Keeping the temperature of the magnesium liquid at 750 ℃ and standing for 20-30 minutes, taking a melt sample for the fourth stokehole component detection, and ensuring that the alloy components are in a set range.
(6) The temperature of the melt is raised to 750-760 ℃, the furnace cover is closed, and the melt is pressurized into the liquid guide pipe by high-purity argon gas to start casting in the crystallizer. The temperature of the tundish is kept between 690 and 700 ℃, the ingot pulling speed of the casting machine is kept between 50 and 200mm/min, and the flow rate of cooling water is kept between 3 and 5m 3 /h。
(7) Peeling the cast ingot, visually detecting that no loose or shrinkage inclusion is visible to naked eyes, and turning the cast ingot to cut the cast ingot into a bar material with the diameter of 65mm multiplied by 150mm for later use according to an extrusion forming process.
(8) Homogenizing the prepared common magnesium alloy rod with the diameter of 65mm multiplied by 150mm under the protection of argon, wherein the homogenizing parameter is 400 ℃, and water quenching is carried out at room temperature for 24 hours.
(9) Adopting a 300T horizontal extruder to extrude and form the homogenized bar material with the diameter of 65mm multiplied by 150mm, wherein the extruded section material is a plate material with the section size of 55 multiplied by 3.5mm, and the temperature of an extrusion die is as follows: 400 ℃, extrusion working speed: 0.3mm/min, extruder barrel temperature setting: 320 ℃, setting of extrusion ratio: 17, adopting a traction machine to draw the extruded material, wherein the traction force is about 200N.
(10) And annealing the comparative common Mg-8Al-0.5Zn-0.2Mn (wt.%) wrought magnesium alloy at the temperature of 420 ℃ for a time period of 4h,7h.
Performance test of common commercial Mg-Al wrought alloy
And (3) carrying out creep property test on the multi-element microalloyed Mg-8Al-0.5Zn-0.2Mn (wt.%) annealed plate by adopting a uniaxial tensile creep test method, and carrying out room-temperature mechanical property test on the plate by adopting a room-temperature uniaxial tensile mechanical property test method. The test results are shown in table 4. It can be seen that the multi-element microalloyed alloy has higher mechanical properties and medium-temperature creep resistance than the common Mg-Al wrought alloy (compare table 1,2,3).
TABLE 4 comparative examples mechanical and creep Property test results
FIG. 1 is a comparison of steady state creep rate and room temperature tensile strength of cast Mg-Al alloys and the creep resistant extruded Mg-Al alloys of the present invention at 100-150 deg.C/50-100 MPa.
The EBSD analysis result in FIG. 2 shows that the grain size of the multi-microalloyed Mg-Al alloy AZ80M (the AZ80M refers to creep-resistant magnesium alloy designed by multi-microalloying in the above example) is more uniform than that of the common commercial AZ80 magnesium alloy (a) the AZ80 plates in the annealing states of 420 ℃/4h and 420 ℃/7h are respectively defined as AZ80 (a) and AZ80 (b), (b) the AZ80M plates in the annealing states of 420 ℃/4h and 420 ℃/7h are respectively defined as AZ80M (a) and AZ80M (b), (c) the grain size distribution histograms of the above four plates in the annealing states, and the orientation schematic diagrams of the inverse pole diagrams of the sample coordinate system and the EBSD are shown in the lower left corner.
Figure 3 shows that the multi-microalloyed Mg-Al alloy AZ80M has higher tensile strength and total elongation at break than the common commercial AZ80 magnesium alloy. In the figure, the AZ80 plates AZ80 (a) and AZ80 (b) in annealing states of 420 ℃/4h and 420 ℃/7h have tensile strength of about 310MPa and total elongation at break of about 15 percent. And the AZ80M (a) and AZ80M (b) of the AZ80M plates in annealing states of 420 ℃/4h and 420 ℃/7h have tensile strength of about 370MPa and total elongation at break of about 19 percent.
Fig. 4 shows that the multi-microalloyed Mg-Al alloy AZ80M has higher basal plane texture strength than the common commercial AZ80 magnesium alloy, (a, c) the AZ80 sheet in the 420 ℃/4h annealed state has basal plane texture strength of 15MRD (MRD is dimensionless unit of relative texture strength), while the AZ80M (a) has basal plane texture strength of 16MRD. In the graph (b, d), the basal plane texture strength of the AZ80 plate in the 420 ℃/7h annealing state is 11MRD, and the basal plane texture strength of the AZ80M (a) is 23MRD. It can be seen that the multielement microalloying promotes the strengthening of the texture of the basal plane of the annealed sheet.
In the graph 5, after the AZ80 magnesium alloy creeps at 125 ℃/50MPa, the DP content of the end gradient stress area and the corresponding Vickers hardness value present gradient change. (a) The DP content increases significantly with increasing stress from the A to B position, and (B) the graph corresponds to the results of the measurement of the DP content and Vickers hardness from the A to B position in the graph (a), it can be seen that Vickers hardness also increases with increasing DP content, and Δ HV is the increase in micro Vickers hardness relative to the as-annealed sheet.
FIG. 6 shows that after 125 ℃/50MPa creep deformation of the multi-element microalloyed AZ80M magnesium alloy, the DP content of the end gradient stress area and the corresponding Vickers hardness value are basically kept stable. (a) The DP content from A to B position is basically stable without significant increase along with the increase of stress, and the Vickers hardness of the graph (B) corresponds to the test results of the DP content from A to B position and the Vickers hardness in the graph (a), and the Vickers hardness has no star change.
Interpretation of terms
Deformation of magnesium alloy:
a classification method for magnesium alloys according to the processing history generally refers to a classification method for obtaining magnesium alloys with obviously improved mechanical strength and structural uniformity by carrying out plastic forming on cast magnesium alloys. The alloy is more suitable for lightweight parts of medium-high strength magnesium alloy.
Micro-alloying:
by selectively adding trace alloy elements (mass content is generally less than 0.5%) to original alloy system, the structure state and performance strength of original alloy can be obviously improved. The microalloying method exhibits better economic applicability due to higher alloying effect and low element content requirement.
Medium temperature creep:
the invention relates to the medium temperature service condition of high-strength magnesium alloy, generally 0.3-0.5T m (T m The melting point of the magnesium alloy) temperature range is referred to as medium temperature creep. For example, for the comparative example AZ80 magnesium alloy of the present invention, 125 ℃ is in its range of medium temperature service conditions.
Minimum creep rate:
the strain rate during the creep process of the material changes with time, when the strain rate has a minimum value, the minimum creep rate of the creep process is called, and generally corresponds to the steady-state creep rate of the second stage, and the method is generally adopted
And (4) showing.
Creep resistance:
the ability of a material to resist creep deformation is generally inversely proportional to the minimum creep rate (or steady state creep rate). The smaller the minimum creep rate, the higher the creep resistance in the corresponding state.
Continuous precipitation and discontinuous precipitation:
the invention relates to a Mg-Al series alloy, in the middle temperature creep process, al solute atom grain boundary diffusion rate is faster than that in the crystal, and the Al solute atom grain boundary diffusion rate is easy to precipitate along the grain boundary with grain boundary migration to form a cellular structure with alpha-Mg and beta-Mg 17Al12 dual-phase lamellar alternate growth, and the alpha-Mg in the growth front edge of the cellular structure and the alpha-Mg matrix orientation at the adjacent side are in a Discontinuous relation, so that the grain boundary precipitation is called Discontinuous precipitation (Discontinuous precipitation), DP for short. Distinguished from Continuous Precipitation (CP) in intragranular formation.
Dynamic precipitation:
the invention relates to a method for separating magnesium-aluminum alloy solid solution from a magnesium-aluminum alloy material, which is characterized in that during a creep process, a magnesium-aluminum alloy solid solution is simultaneously precipitated along with creep deformation, and comprises non-continuous grain boundary precipitation and continuous in-grain precipitation. Distinguished from static ageing without the influence of applied stress and strain.
Deformation texture:
the present invention is especially the phenomenon of crystal grain orientation in cold and hot formed polycrystalline deformed magnesium alloy, which is called preferred orientation, is gathered and distributed along some directions to result in increased orientation probability in these directions.
Electron backscatter diffraction (EBSD):
electron Back-scattered Diffraction (EBSD) enables rapid and accurate measurement of crystal orientation by using the back-scattered Diffraction pattern on each crystal or regularly spaced lattice planes within a crystal grain. The EBSD disclosed by the invention is mainly applied to crystal orientation measurement, micro texture analysis, grain size measurement and the like.
Claims (10)
1. The creep-resistant Mg-Al wrought magnesium alloy is characterized by comprising the following components in percentage by weight: 7 to 9 percent of Al, 0.2 to 0.5 percent of Zn, 0 to 0.5 percent of Y, 0 to 0.4 percent of Ca, 0 to 0.5 percent of Nd, and the balance of Mg.
2. A preparation method of creep-resistant Mg-Al wrought magnesium alloy, which is characterized in that the creep-resistant Mg-Al wrought magnesium alloy based on the claim 1 comprises the following steps:
preparing alloy raw materials and auxiliary materials by adopting a purified magnesium alloy semi-continuous casting system;
gradually adjusting the temperature of a purified magnesium alloy semi-continuous casting system according to a smelting process, adding material adjusting components, then sequentially carrying out high-temperature gradient standing for impurity removal, carrying out secondary adjustment on infinitesimal components, and then carrying out casting and forming;
and carrying out plastic forming treatment on the cast and formed product to obtain the creep-resistant multi-microalloyed Mg-Al deformation alloy.
3. The method for preparing the creep-resistant Mg-Al wrought magnesium alloy according to claim 2, wherein in the purified magnesium alloy semi-continuous casting system, the crucible is made of a high-purity high-density graphite crucible; the catheter adopts a 304 stainless steel pipe; the crystallizer adopts the graphite inner wall; the cooling medium is industrial water.
4. The method for preparing the creep-resistant Mg-Al wrought magnesium alloy according to claim 2, wherein the purity of the alloy raw materials and auxiliary materials is as follows: 99.98% magnesium, 99.994% aluminum, 99.995% zinc; the microalloy elements are added in a master alloy form: 99.9% Mg-30Y, 99.9% Mg-20Ca, 99.9% Mg-30Nd; the flux adopts No. 5 flux: mgCl 2 =46-54%, KCl =29-33%, naCl =17-21%, water-insoluble matter ≤ 1.5%, water content ≤ 1%; the shielding gas was 99.999% argon.
5. The method for preparing the creep-resistant Mg-Al wrought magnesium alloy according to claim 4, wherein the temperature is gradually adjusted by a smelting process, and materials are added at proper time for adjusting the components:
a) Heating up in steps for protection for standby: heating a completely-debugged purified magnesium alloy semi-continuous casting system to 300 ℃ and preserving heat for 2h, introducing argon into an exposed area of a graphite crucible to protect and continuously heating to 600 ℃ and preserving heat for 1h, and then heating to 750 ℃ for later use;
b) Detecting a main element alloy molten material: firstly, casting ingots of magnesium, zinc and aluminum into a crucible according to the alloy proportioning components and the burning loss rate of alloy elements; keeping the temperature at 740-750 ℃ to ensure that all the input materials are melted, stirring the materials in the solution for about 10-15 minutes by adopting argon, and taking a melt sample to perform primary stokehole component detection;
c) Detecting primary refining components: refining the No. 5 flux with the mass ratio of 1-3% of the total melt mass at 740-750 ℃ for 10-15 minutes, stirring the refined flux in the solution by adopting argon, and taking a melt sample to perform secondary stokehole component detection;
d) Adjusting the components of the micro-element alloy: adding magnesium, zinc, aluminum and Mg-30Y, mg-30Nd ingots, adjusting alloy components, then carrying out secondary refining, refining at 740-750 ℃ by using No. 5 flux with the mass ratio of about 1-3% of the total melt mass, and stirring in the solution for about 10-15 minutes by adopting argon gas; and taking a melt sample for carrying out third stokehole component detection to ensure that the components of the micro-element alloy are within a set range.
6. The method for preparing the creep-resistant Mg-Al wrought magnesium alloy according to claim 2, wherein the high-temperature gradient standing is adopted for impurity removal: keeping the temperature of the magnesium liquid at 750 ℃ and standing for 15-20 minutes, then removing slag at the bottom of the crucible, and keeping the temperature of the magnesium liquid at 720-730 ℃ and standing for 10-15 minutes; taking a melt sample for fourth stokehole component detection to ensure that the components of the micro-element alloy are within a set range;
secondary adjustment of the microelement: adding Mg-20Ca ingot at the melt temperature of 720-730 ℃, stirring in the solution for about 2-5 minutes by adopting argon, adjusting the alloy components to be within a set range, and preparing for casting.
7. The method for preparing the creep-resistant Mg-Al wrought magnesium alloy according to claim 2, wherein the casting mold is used for casting and forming: raising the temperature of the melt to 750-760 ℃, closing a furnace cover, and putting the melt into a liquid guide pipe under high-purity argon pressure to start pouring; the temperature of the tundish is kept between 690 and 700 ℃, the ingot pulling speed of the casting machine is kept between 50 and 200mm/min, and the flow rate of cooling water is kept between 3 and 5m 3 And h, peeling the semi-continuous casting rod, carrying out visual detection without loose and shrinkage cavity impurities visible to naked eyes, and cutting the material for later use according to the requirements of a plastic forming process.
8. The method for preparing creep-resistant Mg-Al wrought magnesium alloy according to claim 7, wherein the plastic forming treatment:
a) Homogenizing: homogenizing the scalped multi-element microalloyed Mg-Al alloy cast ingot under the protective atmosphere, wherein the homogenization temperature is 400-420 ℃, the homogenization time is 20-30h, and the cooling mode is water quenching;
b) Plastic forming: performing thermal mechanical treatment on the multi-element microalloyed Mg-Al alloy homogenized cast ingot;
c) Heat treatment after forming: and annealing the multi-element microalloyed Mg-Al wrought magnesium alloy.
9. The method of claim 8, wherein the thermo-mechanical treatment is an extrusion treatment of: temperature of the extrusion die: 350-400 ℃, extrusion working speed: 0.3-1mm/min, setting the temperature of the extrusion cylinder: 300-350 ℃, setting the extrusion ratio: 10-30, and the extrusion discharge is drawn by a tractor, and the traction force is about 100-500N.
10. The method for preparing the creep-resistant Mg-Al wrought magnesium alloy according to claim 8, wherein the annealing temperature is in the range of 300-420 ℃ and the annealing time is 2-8h.
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