CN111593244A - Novel multi-element corrosion-resistant magnesium alloy and preparation method thereof - Google Patents
Novel multi-element corrosion-resistant magnesium alloy and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/115—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by spraying molten metal, i.e. spray sintering, spray casting
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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Abstract
The invention relates to a novel multi-element corrosion-resistant magnesium alloy and a preparation method thereof, wherein alloy raw materials with different percentages are weighed and placed in a graphite crucible, and SF is introduced into a resistance furnace2+CO2Smelting protective gas, preparing a required billet by adopting a spray deposition process, and finally carrying out extrusion plastic forming on the billet to prepare the multi-element corrosion-resistant magnesium alloy containing Al, Sr, Nd and Y. The jet deposition technology adopted by the invention can improve the defects of impurities, uneven components, air holes and the like mixed in the smelting process, and improves the mechanical property and the corrosion resistance of the magnesium alloy by an extrusion plastic forming method. The magnesium alloy prepared by the invention has the advantages of uniform structure, fine crystal grain and excellent mechanicsThe corrosion resistance is high, the operation is easy, the cost is low, the problem that the corrosion rate of the magnesium alloy is too high is solved, and the application of the magnesium alloy is promoted in the engineering environment.
Description
Technical Field
The invention relates to the technical field of non-ferrous metal materials, in particular to a novel multi-element corrosion-resistant magnesium alloy, a spray deposition technology and an extrusion forming process.
Background
The magnesium alloy has a series of advantages of low density, high specific strength, high specific rigidity, good casting performance, good cutting performance, good thermal conductivity and the like, has good application prospect in the fields of transportation, electronics, medicine and military, and is known as the most green and environment-friendly material in the 21 st century, but the standard electrode potential of the magnesium alloy is extremely low, and the magnesium alloy is wet and has the characteristics of high strength, high specific strength, good casting performance, good cutting performance and good heat conductivityUnder the environment, when the magnesium alloy is contacted with other metals, the magnesium alloy is easy to corrode, the generated oxide film can not effectively protect the magnesium alloy, and meanwhile, the oxide film is very easy to react with Cl-、SO4 2-And NO3 -And the like, to dissolve and damage the interior of the magnesium alloy. And in the smelting process, harmful impurity elements are very easy to be doped, so that the corrosivity of the magnesium alloy is greatly increased, and the application of the magnesium alloy is greatly limited. The addition of alloy elements is one of the good means for improving the corrosion resistance of magnesium alloy, the solubility of Al element in Mg element is reduced along with the reduction of temperature, although soft phase Mg is easily formed17Al12The yield strength and creep property at high temperature are deteriorated, but play an important role in improving the corrosion resistance of the magnesium alloy and improve the castability of the magnesium alloy; sr element can refine the structure of the magnesium alloy, improve the high-temperature mechanical property of the magnesium alloy and form Al with high melting point with Al4Sr and Mg8Al4Sr phase to thereby reduce Mg17Al12The number of phases and the generated new phase can reduce the potential difference with the magnesium matrix, thereby improving the corrosion resistance of the magnesium alloy; the addition of Nd and Y rare earth elements can refine grains, strengthen the alloy and form intermetallic compounds containing rare earth with different components, thereby reducing the potential difference between precipitated phases and a magnesium matrix, leading to the weakening of the hydrogen evolution process and further improving the corrosion resistance and the mechanical property of the magnesium alloy.
The processing mode of the magnesium alloy mainly comprises processes of extrusion, rolling, die casting, rapid solidification, powder metallurgy and the like, different processes can also improve the performance of the magnesium alloy, the spray deposition technology is an advanced forming technology integrating the methods of rapid solidification, powder metallurgy and the like, the spray deposition technology is adopted to atomize molten metal flowing out through a flow guide pipe into fine liquid drops, the liquid drops are radiated to obtain a certain supercooling degree, are rapidly solidified on a substrate and are gradually deposited into a large and compact deposition blank. The jet deposition technology has no macroscopic segregation and interfacial reaction, and can also refine the structure of the magnesium alloy, ensure uniform crystal grains and solve the problem of particle reinforced magnesium-based composite material in the traditional sense.
Disclosure of Invention
The invention aims to provide a multi-element corrosion-resistant magnesium alloy containing Al, Sr, Nd and Y and a preparation method thereof, wherein the multi-element corrosion-resistant magnesium alloy utilizes a multi-alloying technology to improve the potential of a magnesium alloy matrix and refine the structure of the magnesium alloy so as to improve the corrosion resistance of the magnesium alloy; the invention provides the multielement reinforced corrosion-resistant magnesium alloy, which has lower manufacturing cost and simple operation.
In order to achieve the aim of the scheme, the invention adopts the technical scheme that.
The multi-element corrosion-resistant magnesium alloy containing Al, Sr, Nd and Y comprises the following components of 5.5-6.5% of Al, 0.8-1.5% of Sr, 0.2-0.8% of Nd, 0.2-1.5% of Y and the balance of Mg and negligible impurity elements such as Fe, Cu and the like in percentage by mass, raw materials are smelted, a blank ingot is prepared by adopting a spray deposition technology, and finally the finished product is obtained by extrusion processing.
The alloying of the present invention has the advantage.
First, the maximum solubility of Al in Mg is 12.7%, forming Mg with Mg17Al12The soft phase is beneficial to improving the corrosion resistance of the magnesium alloy, so that the film on the surface of the magnesium is not easy to be oxidized, thereby improving the corrosion resistance.
Secondly, alkaline earth element Sr added into Mg can not only reduce the supercooling degree, but also reduce the growth speed of crystal grains, thereby refining the crystal grains, simultaneously reducing the solid solubility of Al in a magnesium matrix and reducing the Mg17Al12The quantity of the soft phase and the high melting point Al-Sr new phase are easily formed at the crystal boundary, and on the other hand, the new phase can reduce the potential difference with the matrix phase, enhance the corrosion resistance of the matrix and further reduce the corrosion rate.
Thirdly, rare earth elements Nd and Y are added into the magnesium alloy, thereby not only refining the structureThe melt is purified, the dislocation motion is hindered, the mechanical property of the magnesium alloy is improved, Y, Nd and Mg are both close-packed hexagonal lattices, the atomic radiuses and the lattice constants of the Y, Nd and the Mg are close to each other, the Y, Nd and the Mg are easy to serve as heterogeneous nucleation cores of the magnesium alloy and inhibit the grains from growing, so that the magnesium alloy is refined, and in addition, Nd and Y elements and Al can generate high-melting-point thermally stable Al-Nd phase and Al-Y phase near the grain boundary of the alloy, so that the dislocation motion and the grain boundary slippage are inhibited, and the Mg is inhibited17Al12The phase is separated out, Nd and Y are taken as active rare earth elements and are easy to react with air, so that the advantage of removing impurities is achieved.
A method for forming a multi-element corrosion-resistant magnesium alloy containing Al, Sr, Nd and Y comprises the following steps.
Firstly, placing a graphite crucible into a resistance furnace, preheating to 300 ℃, and preserving heat for 1 hour; putting pure magnesium ingot and pure aluminum ingot into graphite crucible, introducing SF2+CO2Heating protective gas to 720 ℃, and preserving heat for a period of time until the cast ingot is in a molten state; then, raising the furnace temperature to 740-800 ℃, adding Mg-Sr intermediate alloy, stirring by using a stirring rod, standing for 10 minutes, adding Mg-Nd and Mg-Y intermediate alloy into the melt, and stirring; and after the temperature is kept for 30 minutes, slagging off the molten liquid.
Step two, rapidly pouring the molten liquid into a guide funnel for spray deposition, and performing spray deposition under protective gas, wherein the protective gas is N2The pressure of the atomizing gas is 0.6-0.9 MPa, and the flow rate of the atomizing gas is 20-30 m3And/min, wherein the melt flow rate is 5-9 kg/min, and depositing to obtain a magnesium alloy billet.
And step three, processing the material into a bar with the diameter of 40mm, coating a release agent on an extrusion die and a billet before extrusion, putting the bar into a heating furnace to 380 ℃, preserving the heat for 1 hour, and then putting the bar on an extruder with the extrusion speed of 2mm/s and the extrusion ratio of 11:1 for extrusion, thereby obtaining the required multi-element corrosion-resistant magnesium alloy containing Al, Sr, Nd and Y.
The invention achieves the beneficial effects.
Firstly, the determined alloying elements are all cheap and easily-obtained metals, and compared with the alloying of other rare earth elements, the used Nd and Y elements have good biocompatibility, and meanwhile, the composite addition of Nd and Y can obviously improve the high-temperature performance and corrosion resistance of the magnesium alloy.
Secondly, the structure is stable and uniform, the defects of air holes, cracks and the like in the traditional casting process are greatly improved by adopting a spray deposition technology, and the structure is compact and the crystal grains are fine. Through the subsequent forward extrusion process, the density of the magnesium alloy can be improved, and the mechanical property and the corrosion resistance of the magnesium alloy are improved.
Thirdly, the corrosion rate is slowed down, firstly, rare earth elements in alloying can generate new phases with Al, the potential difference with a matrix phase is reduced, the micro-galvanic corrosion of the magnesium alloy is reduced, the corrosion resistance of the magnesium alloy is improved, secondly, the spray deposition technology can inhibit grain boundary segregation, the solubility of each alloying element in a magnesium matrix is improved, the content of a second phase is reduced, the corrosion rate is reduced, finally, forward extrusion can further enable crystal grains to be fine, and the mechanical property of the magnesium alloy material is also improved.
Drawings
FIG. 1 is a graph showing the change in corrosion rate of comparative example 1 and examples 1 to 3.
Detailed Description
The invention provides a multi-element corrosion-resistant magnesium alloy containing Al, Sr, Nd and Y and a preparation method thereof, and the specific implementation mode is as follows.
Comparative example 1.
The magnesium alloy comprises the following components in percentage by mass: 6%, Sr: 1 percent and the balance of Mg, and the preparation process is as follows.
(1) Weighing 72g of Al and 120g of Mg-20Sr intermediate alloy, firstly putting a graphite crucible into a resistance furnace, preheating to 300 ℃, and preserving heat for 1 hour; putting pure magnesium ingot and pure aluminum ingot into graphite crucible, introducing SF2+CO2Heating protective gas to 720 ℃, and preserving heat for a period of time until the cast ingot is in a molten state; then, the furnace temperature is increased to 740-800 ℃, 120g of Mg-30Sr intermediate alloy is added, and the mixture is stirred by a stirring rod and stands for 10 minutes; and after the temperature is kept for 30 minutes, slagging off the molten liquid.
(2) Quickly pouring the molten liquid into the nozzleIn the jet deposition guide funnel, jet deposition is carried out under protective gas, and the protective gas is N2The pressure of the atomizing gas is 0.6MPa, and the flow rate of the atomizing gas is 20m3And/min, the flow rate of the melt is 5kg/min, and a billet of the magnesium alloy is obtained by deposition.
(3) Processing the material into a bar with the diameter of 40mm, coating a release agent on an extrusion die and a billet before extrusion, putting the bar into a heating furnace to 380 ℃ and keeping the temperature for 1 hour, and then putting the bar on an extruder with the extrusion speed of 2mm/s and the extrusion ratio of 11:1 for extrusion, thereby obtaining the required Mg-6Al-1Sr corrosion-resistant magnesium alloy.
Example 1.
The magnesium alloy comprises the following components in percentage by mass: 6%, Sr: 1%, Nd: 0.2%, Y:0.2 percent and the balance of Mg, and the preparation process is as follows.
(1) Weighing 72g of Al, 120g of Mg-20Sr intermediate alloy, 8g of Mg-30Y intermediate alloy and 8g of Mg-30Nd intermediate alloy, firstly putting a graphite crucible into a resistance furnace, preheating to 300 ℃, and preserving heat for 1 hour; putting pure magnesium ingot and pure aluminum ingot into graphite crucible, introducing SF2+CO2Heating protective gas to 720 ℃, and preserving heat for a period of time until the cast ingot is in a molten state; then, raising the furnace temperature to 740-800 ℃, adding 120g of Mg-30Sr intermediate alloy, stirring by using a stirring rod, standing for 10 minutes, adding 8g of Mg-30Nd and 8g of Mg-30Y intermediate alloy into the melt, and stirring; and after the temperature is kept for 30 minutes, slagging off the molten liquid.
(2) Quickly pouring the molten liquid into a guide funnel for spray deposition, and performing spray deposition under protective gas N2The pressure of the atomizing gas is 0.6MPa, and the flow rate of the atomizing gas is 20m3And/min, the flow rate of the melt is 5kg/min, and a billet of the magnesium alloy is obtained by deposition.
(3) Processing the material into a bar with the diameter of 40mm, coating a release agent on an extrusion die and a billet before extrusion, putting the bar into a heating furnace to 380 ℃ and keeping the temperature for 1 hour, and then putting the bar on an extruder with the extrusion speed of 2mm/s and the extrusion ratio of 11:1 for extrusion, thereby obtaining the required Mg-6Al-1Sr-0.8Nd-0.8Y corrosion resistant magnesium alloy.
Example 2.
The magnesium alloy comprises the following components in percentage by mass: 6%, Sr: 1%, Nd: 0.5%, Y: 0.7 percent and the balance of Mg, and the preparation process is as follows.
(1) Weighing 72g of Al, 120g of Mg-20Sr intermediate alloy, 28g of Mg-30Y intermediate alloy and 20g of Mg-30Nd intermediate alloy, firstly putting a graphite crucible into a resistance furnace, preheating to 300 ℃, and preserving heat for one hour; putting pure magnesium ingot and pure aluminum ingot into graphite crucible, introducing SF2+CO2Heating protective gas to 720 ℃, and preserving heat for a period of time until the cast ingot is in a molten state; then, raising the furnace temperature to 740-800 ℃, adding 120g of Mg-30Sr intermediate alloy, stirring by using a stirring rod, standing for 10 minutes, adding 20g of Mg-30Nd and 28g of Mg-30Y intermediate alloy into the melt, and stirring; and after the temperature is kept for 30 minutes, slagging off the molten liquid.
(2) Quickly pouring the molten liquid into a guide funnel for spray deposition, and performing spray deposition under protective gas N2The pressure of the atomizing gas is 0.7MPa, and the flow rate of the atomizing gas is 25m3And/min, the flow rate of the melt is 7kg/min, and a billet of the magnesium alloy is obtained by deposition.
The forward extrusion test of this example was consistent with comparative example 1 and example 1.
Example 3.
The magnesium alloy comprises the following components in percentage by mass: 6%, Sr: 1%, Nd: 0.8%, Y: 1.2 percent and the balance of Mg, and the preparation process is as follows.
(1) Weighing 72g of Al, 120g of Mg-20Sr intermediate alloy, 46g of Mg-30Y intermediate alloy and 32g of Mg-30Nd intermediate alloy, firstly putting a graphite crucible into a resistance furnace, preheating to 300 ℃, and preserving heat for 1 hour; putting pure magnesium ingot and pure aluminum ingot into graphite crucible, introducing SF2+CO2Heating protective gas to 720 ℃, and preserving heat for a period of time until the cast ingot is in a molten state; then, raising the furnace temperature to 740-800 ℃, adding 120g of Mg-30Sr intermediate alloy, stirring by using a stirring rod, standing for 10 minutes, adding 32g of Mg-30Nd and 46g of Mg-30Y intermediate alloy into the melt, and stirring; after 30 minutes of heat preservation, the molten liquid is processedAnd (6) slagging off.
(2) Quickly pouring the molten liquid into a guide funnel for spray deposition, and performing spray deposition under protective gas N2The pressure of the atomizing gas is 0.8MPa, and the flow rate of the atomizing gas is 30m3And/min, the flow rate of the melt is 9kg/min, and a billet of the magnesium alloy is obtained by deposition.
The forward extrusion test of this example was identical to comparative example 1 and example 1.
According to the invention, alloying, spray deposition and forward extrusion are combined, compared with the traditional method, the corrosion resistance of the magnesium alloy is obviously improved, and in order to further illustrate the result, the corrosion rate of the Mg-Al-Sr-Nd-Y alloy obtained in comparative example 1 and examples 1-3 of the invention in a 3.5% NaCl solution is tested; the result shows that the corrosion resistance of the Mg-Al-Sr-Nd-Y alloy provided by the invention is obviously improved.
Claims (6)
1. A novel multi-element corrosion-resistant magnesium alloy and a preparation method thereof are characterized in that the magnesium alloy comprises the following chemical components of, by mass, 5.5-6.5% of Al, 0.8-1.5% of Sr, 0.3-0.8% of Nd, 0.3-1.5% of Y and the balance of Mg and negligible impurity elements such as Fe, Cu and the like, raw materials are smelted, a blank ingot is prepared by adopting a spray deposition technology, and finally the raw materials are extruded to form a finished product.
2. The novel multi-element corrosion-resistant magnesium-containing alloy and the preparation method thereof according to claim 1, wherein the corrosion-resistant magnesium-containing alloy is characterized in that: sr, Nd and Y are added in the form of Mg-Sr, Mg-Nd and Mg-Y intermediate alloy.
3. The novel multi-element corrosion-resistant magnesium alloy and the preparation method thereof as claimed in claim 1, wherein the smelting comprises the following steps:
(1) the experimental materials are pure magnesium ingot, pure aluminum ingot, Mg-Sr, Mg-Nd and Mg-Y intermediate alloy respectively; the raw materials are polished by abrasive paper, so that the doping of oxides is prevented, and the defects caused during smelting are reduced;
(2) smelting: placing the graphite crucible into an electric fieldPreheating to 300 ℃ in a resistance furnace, and preserving heat for 1 hour; putting pure magnesium ingot and pure aluminum ingot into graphite crucible, introducing SF2+CO2Heating protective gas to 720 ℃, and preserving heat for a period of time until the cast ingot is in a molten state; then, raising the furnace temperature to 740-800 ℃, adding Mg-Sr intermediate alloy, stirring by using a stirring rod, standing for 10 minutes, adding Mg-Nd and Mg-Y intermediate alloy into the melt, and stirring; after the temperature is kept for 30 minutes, the melt is subjected to slagging off, the melt is rapidly poured into a guide funnel for jet deposition, and then the material is subjected to subsequent processing treatment.
4. The novel multi-element corrosion-resistant magnesium alloy and the preparation method thereof according to claim 1, wherein the atomizing gas in the spray deposition process is nitrogen.
5. The novel multi-element corrosion-resistant magnesium alloy and the preparation method thereof as claimed in claim 4, wherein the pressure of the atomizing gas is 0.6-0.9 MPa, and the flow rate of the atomizing gas is 20-30 m3The melt flow rate is 5-9 kg/min.
6. The novel multi-element corrosion-resistant magnesium alloy and the preparation method thereof according to claim 1, wherein the novel multi-element corrosion-resistant magnesium alloy is obtained by processing the central part of an alloy billet into a bar with the diameter of 40mm by adopting a forward hot extrusion mode and an extrusion ratio of 11:1, wherein the extrusion speed is 2mm/s, and extruding at 380 ℃.
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| WO2022267488A1 (en) * | 2021-06-25 | 2022-12-29 | 江苏大学 | Preparation method for high-toughness corrosion-resistant az80 magnesium alloy |
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Application publication date: 20200828 |