CN114540653A - High-corrosion-resistance magnesium alloy processing technology - Google Patents
High-corrosion-resistance magnesium alloy processing technology Download PDFInfo
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- CN114540653A CN114540653A CN202210171272.2A CN202210171272A CN114540653A CN 114540653 A CN114540653 A CN 114540653A CN 202210171272 A CN202210171272 A CN 202210171272A CN 114540653 A CN114540653 A CN 114540653A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D43/00—Mechanical cleaning, e.g. skimming of molten metals
- B22D43/001—Retaining slag during pouring molten metal
- B22D43/004—Retaining slag during pouring molten metal by using filtering means
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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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
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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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/12—Light metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/30—Anodisation of magnesium or alloys based thereon
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a high corrosion resistance magnesium alloy processing technology, which comprises the steps of preheating a crucible to 200-300 ℃, introducing protective gas, adding a pure magnesium ingot into the crucible, heating the crucible to 720-750 ℃, and melting the pure magnesium ingot into magnesium liquid; adding aluminum ingots, zinc ingots, tin ingots, Mg-Si intermediate alloys, Mg-Sr intermediate alloys and Ca which are preheated to 200-250 ℃ in protective gas into the magnesium liquid, mixing and stirring the mixture, and completely melting the mixture to obtain magnesium alloy melt; introducing the magnesium alloy melt into an ingot mold preheated to 250-300 ℃, and cooling and molding in protective gas; soaking the surface of the magnesium alloy block in a hydrofluoric acid solution for a period of time, cleaning the surface of the magnesium alloy block by using deionized water, carrying out anodic oxidation in an electrolyte of ammonium phosphate to form a protective film on the surface of the magnesium alloy block, and cleaning the protective film by using the deionized water; and coating a layer of sol isolation solution on the protective film, and drying.
Description
Technical Field
The invention relates to the field of magnesium alloy manufacturing, in particular to a high-corrosion-resistance magnesium alloy processing technology.
Background
The magnesium alloy is an alloy formed by adding other elements on the basis of magnesium. The magnesium alloy is characterized in that: the aluminum alloy has the advantages of small density, high strength, large elastic modulus, good heat dissipation, good shock absorption, larger impact load bearing capacity than aluminum alloy, and good organic matter and alkali corrosion resistance. The main alloy elements in the magnesium alloy comprise aluminum, zinc, manganese, cerium, thorium and a small amount of zirconium or cadmium. The most widely used are magnesium-aluminum alloys, followed by magnesium-manganese alloys and magnesium-zinc-zirconium alloys. The method is mainly used in aviation, aerospace, transportation, chemical engineering, rocket and other industrial departments. The heat dissipation of the magnesium alloy has absolute advantages compared with the heat dissipation of the aluminum alloy, and for the heat dissipater of the magnesium alloy and the aluminum alloy material with the same volume and shape, the heat generated by the heat source is easier to be transferred from the root part of the heat dissipation fin to the top part of the magnesium alloy than the aluminum alloy, and the top part of the magnesium alloy is easier to reach high temperature. Namely, the temperature difference between the root part and the top part of the radiator made of the aluminum alloy material is smaller than that of the radiator made of the magnesium alloy material. This means that the difference between the air temperature at the root and the air temperature at the top of the fin made of a magnesium alloy material is larger than that of the fin made of an aluminum alloy material, and therefore, the diffusion convection of the air inside the radiator is accelerated, and the heat radiation efficiency is improved.
However, after the magnesium alloy ingot is manufactured, oxidation reaction is easy to occur, and corrosion is easy to occur. The waste of magnesium alloy is caused, the production cost of enterprises is increased, the utilization rate of the magnesium alloy is reduced, and the waste of magnesium resource is caused.
Disclosure of Invention
Therefore, it is necessary to provide a processing technology of a high corrosion resistance magnesium alloy aiming at the technical problems that the traditional watch case surface and inside smoothing technology is easy to damage the watch case and the defective rate is high.
A high corrosion resistance magnesium alloy processing technology comprises the following steps:
a magnesium ingot melting step: preheating a crucible to 200-300 ℃, introducing protective gas, adding an antirust agent into the crucible, adding a pure magnesium ingot into the crucible, heating the crucible to 720-750 ℃, and melting the pure magnesium ingot into magnesium liquid;
an element adding step: adding aluminum ingots, zinc ingots, tin ingots, Mg-Si intermediate alloys, Mg-Sr intermediate alloys and Ca which are preheated to 200-250 ℃ in protective gas into magnesium liquid, mixing and stirring, adding a slag-removing agent in the stirring process, and completely melting to obtain magnesium alloy molten liquid;
pouring and cooling: introducing the magnesium alloy melt into an ingot mold preheated to 250-300 ℃, and cooling and molding in protective gas;
a protective film manufacturing step: soaking the surface of the magnesium alloy block in a hydrofluoric acid solution for a period of time, cleaning the surface of the magnesium alloy block by using deionized water, carrying out anodic oxidation in an electrolyte of ammonium phosphate to form a protective film on the surface of the magnesium alloy block, and cleaning the protective film by using the deionized water;
strengthening the protective film: and coating a layer of sol isolation solution on the protective film, and drying to cover a layer of isolation film on the protective film.
In one embodiment, in the magnesium ingot melting step, the protective gas is a mixture of CO2 and SF6 in a volume ratio of 5: 2.
In one embodiment, before the pouring and cooling step, the magnesium alloy melt is filtered to remove impurities in the magnesium alloy melt.
In one embodiment, the filtration is accomplished in a ceramic filter using counter-pressure gas inversion.
In one embodiment, in the element adding step, the slag removing agent comprises the following components in parts by mass: 30 to 50 parts of potassium chloride, 20 to 40 parts of potassium magnesium and 30 to 40 parts of potassium fluoroaluminate.
In one embodiment, in the step of strengthening the protective film, the sol spacer fluid comprises the following components in parts by mass: 45-70 parts of modified silicon dioxide solution, 5-10 parts of epoxy silane cross-linking agent, 8-15 parts of ethylene glycol, 10-20 parts of ethyl acetate, 1-3 parts of calcium carbonate, 5-12 parts of polyurethane adhesive and 5-12 parts of epoxy resin.
In one embodiment, in the protective film strengthening step, the sol spacer fluid further comprises 0.2 to 0.8 parts of a dispersant.
In one embodiment, in the protective film strengthening step, the sol spacer fluid further comprises 0.2 to 0.5 parts of an antifoaming agent.
In one embodiment, in the step of strengthening the protective film, the sol spacer fluid further comprises 0.1 to 0.3 parts of a leveling agent.
In one embodiment, the obtained magnesium alloy contains 5 to 8% of Si, 2 to 3% of Sr, 1.2 to 1.4% of Ca, 1 to 1.8% of Zn, 3 to 5% of Al, 1.5 to 2.8% of SnC, and the balance of Mg
The processing technology of the high-corrosion-resistance magnesium alloy has the advantages that the steps are simple and exquisite, the operation and the control are easy, each step is carefully and minutely carried out, and the protective gas and the antirust agent which are introduced in the magnesium ingot melting step can effectively inhibit the oxidation reaction of the pure magnesium ingot in the high-temperature melting process. Preheating the aluminum ingot, the zinc ingot, the tin ingot, the Mg-Si intermediate alloy, the Mg-Sr intermediate alloy and the Ca in the protective gas, so that the aluminum ingot, the zinc ingot, the tin ingot, the Mg-Si intermediate alloy, the Mg-Sr intermediate alloy and the Ca can be prevented from generating oxidation reaction in the high-temperature melting process. The slag removing agent can effectively separate metal oxide generated in the processing process from the alloy liquid, and the purity of the alloy liquid is improved. The weak acid of hydrofluoric acid solution can remove the easily oxidized calcium on the surface of the alloy block, and then the protective film is formed on the surface of the alloy block through electrolysis. The isolating film further effectively isolates the protective film, and further plays a role in protecting the alloy block. The alloy block supported by the high-corrosion-resistance magnesium alloy processing technology has extremely high corrosion resistance and can be stored for a long time.
Drawings
FIG. 1 is a schematic flow chart of a high corrosion resistance magnesium alloy processing process in one embodiment.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, the present invention provides a high corrosion resistance magnesium alloy processing technology, including the following steps:
step 101: a magnesium ingot melting step: preheating a crucible to 200-300 ℃, introducing protective gas, adding an antirust agent into the crucible, adding a pure magnesium ingot into the crucible, heating the crucible to 720-750 ℃, and melting the pure magnesium ingot into magnesium liquid;
specifically, the crucible is preheated to 200 ℃ to 300 ℃ and then protective gas is introduced, and the crucible can be replaced by other heating containers. Preheating the crucible and improving the heating efficiency, avoiding the cracking of the crucible due to the overlarge temperature difference, and then primarily preheating the pure magnesium ingot. Adding an antirust agent into the crucible, adding a pure magnesium ingot into the crucible, and heating the crucible to 720-750 ℃ to melt the pure magnesium ingot into magnesium liquid; the introduced protective gas and the rust inhibitor can effectively inhibit the oxidation reaction of the pure magnesium ingot in the high-temperature melting process. In the embodiment, the protective gas is a gas formed by mixing CO2 and SF6 according to a volume ratio of 5: 2.
Step 102: element adding step: adding aluminum ingots, zinc ingots, tin ingots, Mg-Si intermediate alloys, Mg-Sr intermediate alloys and Ca which are preheated to 200-250 ℃ in protective gas into magnesium liquid, mixing and stirring, adding a slag-removing agent in the stirring process, and completely melting to obtain magnesium alloy molten liquid;
specifically, aluminum ingots, zinc ingots, tin ingots, Mg-Si intermediate alloys, Mg-Sr intermediate alloys and Ca preheated to 200-250 ℃ in protective gas are added into magnesium liquid, and the aluminum ingots, the zinc ingots, the tin ingots, the Mg-Si intermediate alloys, the Mg-Sr intermediate alloys and the Ca are preheated in the protective gas, so that the aluminum ingots, the zinc ingots, the tin ingots, the Mg-Si intermediate alloys, the Mg-Sr intermediate alloys and the Ca are prevented from generating oxidation reaction while strong bursting in the adding process due to overlarge temperature difference is avoided. Mixing and stirring all elements and the magnesium liquid, adding a slag-removing agent in the stirring process, and completely melting to obtain a magnesium alloy molten liquid; the slag removing agent can effectively separate metal oxide generated in the processing process from the alloy liquid, and the purity of the alloy liquid is improved. In this embodiment, in the element adding step, the slag removing agent includes the following components in parts by mass: 30 to 50 parts of potassium chloride, 20 to 40 parts of potassium magnesium and 30 to 40 parts of potassium fluoroaluminate.
Step 103: pouring and cooling: introducing the magnesium alloy melt into an ingot mold preheated to 250-300 ℃, and cooling and molding in protective gas;
specifically, introducing the magnesium alloy melt into an ingot mold preheated to 250-300 ℃, and cooling and molding in protective gas; the magnesium alloy melt is cooled and formed in the protective gas, so that the magnesium alloy melt is prevented from generating oxidation reaction in the cooling process. The ingot mould is preheated, so that severe bursting of the high-temperature magnesium alloy melt in the casting process is avoided. In this embodiment, before the pouring and cooling step, the magnesium alloy melt is filtered to remove impurities in the magnesium alloy melt, so as to further improve the purity of the magnesium alloy melt. Specifically, in this example, filtration was accomplished in a ceramic filter using counter-pressure gas inversion. In one embodiment, the obtained magnesium alloy contains 5 to 8% of Si, 2 to 3% of Sr, 1.2 to 1.4% of Ca, 1 to 1.8% of Zn, 3 to 5% of Al, 1.5 to 2.8% of SnC, and the balance of Mg
Step 104: a protective film manufacturing step: soaking the surface of the magnesium alloy block in a hydrofluoric acid solution for a period of time, cleaning the surface of the magnesium alloy block by using deionized water, carrying out anodic oxidation in an electrolyte of ammonium phosphate to form a protective film on the surface of the magnesium alloy block, and cleaning the protective film by using the deionized water.
Specifically, the surface of the magnesium alloy block is soaked in a hydrofluoric acid solution for treatment for a period of time, and the hydrofluoric acid solution which is a weak acid can remove calcium which is easy to oxidize on the surface of the alloy block and simultaneously can prevent other metals from being oxidized. It should be noted that calcium is easily oxidized, and if calcium is first oxidized in the magnesium alloy, it corrodes other surrounding metals, which greatly reduces the corrosion resistance of the magnesium alloy, so that calcium on the surface of the magnesium alloy mass is removed first. After the hydrofluoric acid solution is treated, the surface of the magnesium alloy block is cleaned by deionized water, anodic oxidation is carried out in the electrolyte of ammonium phosphate, so that a protective film is formed on the surface of the magnesium alloy block, and the protective film is cleaned by the deionized water. The protective film formed on the surface of the magnesium alloy block has excellent corrosion resistance, and the magnesium alloy block can be well stored.
Step 105: strengthening the protective film: and coating a layer of sol isolation solution on the protective film, and drying to cover a layer of isolation film on the protective film.
Specifically, a layer of sol isolation liquid is coated on the protective film, the sol isolation liquid fills gaps on the protective film, and the sol isolation liquid forms a layer of isolation film on the protective film after drying treatment. In this embodiment, in the step of strengthening the protective film, the sol barrier solution includes the following components in parts by mass: 45-70 parts of modified silicon dioxide solution, 5-10 parts of epoxy silane cross-linking agent, 8-15 parts of ethylene glycol, 10-20 parts of ethyl acetate, 1-3 parts of calcium carbonate, 5-12 parts of polyurethane adhesive and 5-12 parts of epoxy resin. In order to increase the mixing uniformity of the components in the sol spacer fluid, in one embodiment, the sol spacer fluid further comprises 0.2 to 0.8 part of a dispersing agent, and the dispersing agent can enable the components in the sol spacer fluid to be uniformly mixed. The method avoids bubbles generated in the mixing process of the components in the sol spacer fluid and simultaneously avoids bubbles generated in the use process of the sol spacer fluid. In one embodiment, the sol spacer fluid further comprises 0.2 to 0.5 parts of an antifoaming agent. In order to prevent the sol spacer fluid from being uniformly coated on the surface of the magnesium alloy block, in one embodiment, in the protective film strengthening step, the sol spacer fluid further includes a leveling agent in an amount of 0.1 to 0.3 parts. The leveling agent can enable the sol isolation liquid to be uniformly coated on the surface of the magnesium alloy block.
The processing technology of the high-corrosion-resistance magnesium alloy has the advantages that the steps are simple and exquisite, the operation and the control are easy, each step is carefully and minutely carried out, and the protective gas and the antirust agent which are introduced in the magnesium ingot melting step can effectively inhibit the oxidation reaction of the pure magnesium ingot in the high-temperature melting process. Preheating the aluminum ingot, the zinc ingot, the tin ingot, the Mg-Si intermediate alloy, the Mg-Sr intermediate alloy and the Ca in the protective gas, so that the aluminum ingot, the zinc ingot, the tin ingot, the Mg-Si intermediate alloy, the Mg-Sr intermediate alloy and the Ca can be prevented from generating oxidation reaction in the high-temperature melting process. The slag removing agent can effectively separate metal oxide generated in the processing process from the alloy liquid, and the purity of the alloy liquid is improved. The weak acid of hydrofluoric acid solution can remove the easily oxidized calcium on the surface of the alloy block, and then the protective film is formed on the surface of the alloy block through electrolysis. The isolating film further effectively isolates the protective film, and further plays a role in protecting the alloy block. The alloy block supported by the high corrosion resistance magnesium alloy processing technology has extremely high corrosion resistance and can be stored for a long time.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The processing technology of the high-corrosion-resistance magnesium alloy is characterized by comprising the following steps of:
a magnesium ingot melting step: preheating a crucible to 200-300 ℃, introducing protective gas, adding an antirust agent into the crucible, adding a pure magnesium ingot into the crucible, heating the crucible to 720-750 ℃, and melting the pure magnesium ingot into magnesium liquid;
element adding step: adding aluminum ingots, zinc ingots, tin ingots, Mg-Si intermediate alloys, Mg-Sr intermediate alloys and Ca which are preheated to 200-250 ℃ in protective gas into magnesium liquid, mixing and stirring, adding a slag-removing agent in the stirring process, and completely melting to obtain magnesium alloy molten liquid;
pouring and cooling: introducing the magnesium alloy melt into an ingot mold preheated to 250-300 ℃, and cooling and molding in protective gas;
a protective film manufacturing step: soaking the surface of the magnesium alloy block in a hydrofluoric acid solution for a period of time, cleaning the surface of the magnesium alloy block by using deionized water, carrying out anodic oxidation in an electrolyte of ammonium phosphate to form a protective film on the surface of the magnesium alloy block, and cleaning the protective film by using the deionized water;
strengthening the protective film: and coating a layer of sol isolation solution on the protective film, and drying to cover a layer of isolation film on the protective film.
2. The process according to claim 1, wherein in the magnesium ingot melting step, the shielding gas is a mixture of CO2 and SF6 at a volume ratio of 5: 2.
3. The process of claim 1, wherein the magnesium alloy melt is filtered to remove impurities from the magnesium alloy melt prior to the pouring and cooling step.
4. A process according to claim 3, wherein the filtration is accomplished in a ceramic filter by counter-pressure gas-liquid-inversion.
5. The process according to claim 1, wherein in the element addition step, the slag former comprises the following components in parts by mass: 30 to 50 parts of potassium chloride, 20 to 40 parts of potassium magnesium and 30 to 40 parts of potassium fluoroaluminate.
6. The process according to claim 1, wherein in the protective film strengthening step, the sol spacer fluid comprises the following components in parts by mass: 45-70 parts of modified silicon dioxide solution, 5-10 parts of epoxy silane cross-linking agent, 8-15 parts of glycol, 10-20 parts of ethyl acetate, 1-3 parts of calcium carbonate, 5-12 parts of polyurethane adhesive and 5-12 parts of epoxy resin.
7. The process according to claim 6, wherein in the protective film strengthening step, the sol spacer further comprises 0.2 to 0.8 parts of a dispersant.
8. The process according to claim 6, wherein in the protective film strengthening step, the sol spacer fluid further comprises 0.2 to 0.5 parts of an antifoaming agent.
9. The process according to claim 6, wherein in the step of strengthening the protective film, the sol-barrier liquid further comprises 0.1 to 0.3 parts of a leveling agent.
10. The process according to claim 1, wherein the magnesium alloy is obtained with a Si content of 5 to 8%, a Sr content of 2 to 3%, a Ca content of 1.2 to 1.4%, a Zn content of 1 to 1.8%, an Al content of 3 to 5% and a sn content of 1.5 to 2.8%, the balance being Mg.
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