WO2022267488A1 - Preparation method for high-toughness corrosion-resistant az80 magnesium alloy - Google Patents

Preparation method for high-toughness corrosion-resistant az80 magnesium alloy Download PDF

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WO2022267488A1
WO2022267488A1 PCT/CN2022/075860 CN2022075860W WO2022267488A1 WO 2022267488 A1 WO2022267488 A1 WO 2022267488A1 CN 2022075860 W CN2022075860 W CN 2022075860W WO 2022267488 A1 WO2022267488 A1 WO 2022267488A1
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Prior art keywords
magnesium alloy
treatment
micro
arc oxidation
corrosion
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PCT/CN2022/075860
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French (fr)
Chinese (zh)
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唐玲玲
王楠
郭孟
傅嘉琳
韩贞毅
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江苏大学
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Publication of WO2022267488A1 publication Critical patent/WO2022267488A1/en

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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/002—Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C31/00—Control devices, e.g. for regulating the pressing speed or temperature of metal; Measuring devices, e.g. for temperature of metal, combined with or specially adapted for use in connection with extrusion presses
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • 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
    • C25D11/026—Anodisation with spark discharge
    • 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

Definitions

  • the invention relates to the technical field of magnesium alloys, in particular to a preparation method of a strong, tough and corrosion-resistant AZ80 magnesium alloy.
  • magnesium alloy is one of the lightest metal structural materials, and is known as "green engineering material in the 21st century". At the same time, magnesium alloy also has high specific strength and specific stiffness, good With the advantages of castability and dimensional stability, high damping, good electromagnetic interference shielding performance and high recycling rate, it is widely used in aerospace, electronic communication, vehicle manufacturing and national defense technology and other fields.
  • AZ80 magnesium alloy shows excellent mechanical properties.
  • steel, aluminum alloy and other metals due to the special hexagonal close-packed lattice structure of magnesium alloy, it can be activated at room temperature.
  • the slip system is very limited, resulting in poor toughness and low strength at room temperature, making it difficult to deform and process, which severely restricts the development of AZ80 magnesium alloys. Therefore, it is of great significance to develop high-performance AZ80 magnesium alloys.
  • the chemical properties of magnesium are relatively active, and its standard electrode potential is -2.37V. Therefore, even if an oxide film is formed on the surface of the AZ80 magnesium alloy in the natural environment, it cannot effectively protect the metal substrate from harsh conditions such as high temperature and high salt spray. Corrosion occurs in the environment, which also limits the application of AZ80 magnesium alloy in industry.
  • the object of the present invention is to provide a method for preparing a strong, tough and corrosion-resistant AZ80 magnesium alloy.
  • the AZ80 magnesium alloy prepared by the preparation method provided by the present invention has good strength and toughness and excellent corrosion resistance.
  • the invention provides a preparation method of a tough and corrosion-resistant AZ80 magnesium alloy, comprising the following steps:
  • AZ80 magnesium alloy melt is subjected to spray atomization deposition treatment to obtain deposited state AZ80 magnesium alloy ingot;
  • the as-deposited AZ80 magnesium alloy ingot obtained in the step (1) is subjected to homogenization treatment, equal channel angular extrusion deformation and micro-arc oxidation treatment sequentially to obtain a strong, tough and corrosion-resistant AZ80 magnesium alloy.
  • the spray temperature of the spray atomization deposition treatment in the step (1) is 740-760° C., and the spray angle is 10-30°.
  • the atomization pressure of the spray atomization deposition treatment in the step (1) is 0.5-0.7 MPa, and the gas-liquid flow rate ratio is 1.6-1.8.
  • the rotational speed of the receiving tray in the spray atomization deposition treatment in the step (1) is 30-60 rpm, and the descending speed of the receiving tray is 2-5 mm/s.
  • the temperature of the homogenization treatment in the step (2) is 360-400° C.
  • the time of the homogenization treatment is 12-16 hours.
  • the temperature of the medium-channel angular extrusion deformation in the step (2) is 250-300° C.
  • the speed is 2-4 mm/min
  • the number of passes is 6, 10 or 12.
  • the process route of medium channel angular extrusion deformation in the step (2) is B C , and the back pressure is 160-180 MPa.
  • the applied voltage of the micro-arc oxidation treatment in the step (2) is 380-420V
  • the duty ratio is 15-30%
  • the frequency is 400-600Hz
  • the time is 20-25min.
  • the electrolyte composition of the micro-arc oxidation treatment in the step (2) includes: Na 2 SiO 3 15-20g/L, NaOH 25-30g/L, Na 2 B 4 O 7 25-30g/L and magnetic Nickel powder 4g/L.
  • the AZ80 magnesium alloy in the step (1) includes the following components in mass percentage: Al 7.89-8.85%, Zn 0.39-0.50%, Mn 0.23-0.50%, Cu 0.05-0.1%, Si 0.02 ⁇ 0.05%, Fe 0.01 ⁇ 0.03%, the balance is Mg.
  • the invention provides a method for preparing a strong, tough and corrosion-resistant AZ80 magnesium alloy, comprising the following steps: performing spray atomization deposition treatment on an AZ80 magnesium alloy melt to obtain a deposited AZ80 magnesium alloy ingot; The alloy ingot was subjected to homogenization treatment, equal channel angular extrusion deformation and micro-arc oxidation treatment in sequence to obtain a strong, tough and corrosion-resistant AZ80 magnesium alloy.
  • the invention avoids dendrite segregation and coarse structure of the alloy by adopting atomized deposition treatment, avoids the contact of the alloy with oxygen, and reduces the degree of oxidation of the alloy; by adopting equal channel angle extrusion deformation, the crystal grains can be refined, Improve material toughness, and the ultra-fine grain microstructure formed after equal channel angular extrusion deformation can improve the film formation process of micro-arc oxidation treatment, and improve the compactness of the oxide film on the alloy surface; by adopting micro-arc oxidation treatment on the surface of AZ80 magnesium alloy A ceramic layer is formed, and the surface of the ceramic layer has a micron-scale porous structure, which is beneficial to improving the corrosion resistance of the alloy.
  • the AZ80 magnesium alloy provided by the present invention has a tensile strength of 347 MPa, a tensile elongation at break of 12.5%, a full immersion corrosion rate of 3.5 ⁇ 10 -4 mg ⁇ cm -2 h -1 , and a corrosion rate of
  • the current density is 0.7041 ⁇ A/cm 2
  • the impedance value is 8082000 ohms ⁇ cm 2 .
  • the invention provides a preparation method of a tough and corrosion-resistant AZ80 magnesium alloy, comprising the following steps:
  • AZ80 magnesium alloy melt is subjected to spray atomization deposition treatment to obtain deposited state AZ80 magnesium alloy ingot;
  • the as-deposited AZ80 magnesium alloy ingot obtained in the step (1) is subjected to homogenization treatment, equal channel angular extrusion deformation and micro-arc oxidation treatment sequentially to obtain a strong, tough and corrosion-resistant AZ80 magnesium alloy.
  • the AZ80 magnesium alloy melt is subjected to spray atomization deposition treatment to obtain a deposited AZ80 magnesium alloy ingot.
  • the invention avoids dendrite segregation and coarse structure of the alloy by adopting atomization deposition treatment, avoids the contact of the alloy with oxygen, reduces the degree of oxidation of the alloy, is beneficial to improve the strength and corrosion resistance of the alloy, and has a simple process , low cost and improved production efficiency.
  • the present invention has no special limitation on the composition and source of the AZ80 magnesium alloy, and the preparation method of the strong and corrosion-resistant AZ80 magnesium alloy provided by the present invention is applicable to the AZ80 magnesium alloy well known to those skilled in the art.
  • the AZ80 magnesium alloy preferably includes the following components in mass percentage: Al 7.89-8.85%, Zn 0.39-0.50%, Mn 0.23-0.50%, Cu 0.05-0.1%, Si 0.02-0.05% , Fe 0.01-0.03%, the balance is Mg, more preferably Al7.89%, Zn 0.39%, Mn 0.23%, Cu 0.05%, Si 0.02%, Fe 0.01%, and the balance is Mg.
  • the spray temperature of the spray atomization deposition treatment is preferably 740-760°C, more preferably 750-760°C; the spray angle is preferably 10-30°, more preferably 20-30°; the atomization medium It is preferably high-purity nitrogen; the atomization pressure is preferably 0.5-0.7MPa, more preferably 0.6-0.7MPa; the gas-liquid flow rate ratio is preferably 1.6-1.8, more preferably 1.6; the speed of the receiving plate is preferably 30-60rpm, more preferably 50-60 rpm; the lowering speed of the receiving tray is preferably 2-5 mm/s, more preferably 4-5 mm/s.
  • the process parameters of the spray atomization deposition treatment are preferably controlled within the above range, which is beneficial to obtain a densified AZ80 magnesium alloy ingot with a uniform structure.
  • the present invention preferably removes the skin and burrs of the deposited AZ80 magnesium alloy ingot, and makes an ingot with a size of 18mm ⁇ 18mm ⁇ 60mm.
  • the method for preparing the ingot is preferably wire electric discharge cutting.
  • the invention sequentially performs homogenization treatment, equal channel angular extrusion deformation and micro-arc oxidation treatment on the deposited AZ80 magnesium alloy billet to obtain a strong, tough and corrosion-resistant AZ80 magnesium alloy.
  • the temperature of the homogenization treatment is preferably 360-400° C., more preferably 380-390° C.; the time of the homogenization treatment is preferably 12-16 hours, more preferably 14-15 hours.
  • the present invention has no special limitation on the specific operation of the homogenization treatment, and the technical scheme of homogenization treatment well known to those skilled in the art can be adopted.
  • the invention homogenizes the composition of the alloy ingot through homogenization treatment, and eliminates composition segregation and structure inhomogeneity.
  • the homogenized AZ80 magnesium alloy is preferably placed in a lubricant-lubricated equal channel angular extrusion deformation mold for heat preservation treatment, and then the equal channel angular extrusion deformation is performed.
  • the lubricant preferably includes molybdenum disulfide or a mixture of graphite powder and kerosene, more preferably a mixture of graphite powder and kerosene;
  • the temperature of the heat preservation treatment is preferably 150-300°C, more preferably 230- 280° C.;
  • the time for heat preservation treatment is preferably 10 to 20 minutes, more preferably 20 minutes.
  • the temperature of the equal channel angular extrusion deformation is preferably 250-300°C, more preferably 250-280°C;
  • the speed of the equal channel angular extrusion deformation is preferably 2-4mm/min, more preferably It is 2mm/min.
  • the number of passes of the equal channel angular extrusion deformation is preferably 6, 10 or 12 times, more preferably 10 or 12 times.
  • the number of passes of the equal channel angular extrusion deformation is preferably controlled within the above range, which is beneficial to improving the uniformity of the tissue.
  • the present invention adopts equal channel angular extrusion deformation to refine crystal grains and improve material toughness, and the ultra-fine grain microstructure formed after equal channel angular extrusion deformation can improve the film forming process of micro-arc oxidation treatment and improve the oxidation film on the surface of the alloy. The compactness, thereby improving the corrosion resistance of AZ80 magnesium alloy.
  • the process route of the equal channel angular extrusion deformation is preferably B C ; the present invention adopts the Bc process route, and the sample is rotated by 90° between adjacent extrusion passes, which is beneficial to improve the uniformity of the structure.
  • the back pressure of the equal channel angular extrusion deformation is preferably 160-180 MPa, more preferably 170-180 MPa.
  • the back pressure of the equal channel angular extrusion deformation is used to adjust the pressure balance in the mold, and controlling it within the above range is beneficial to make the plastic deformation more stable.
  • the AZ80 magnesium alloy deformed by equal channel angular extrusion is preferably cut, polished, polished and cleaned in sequence, and then subjected to micro-arc oxidation treatment.
  • the present invention has no special limitation on the operations of cutting, grinding, polishing and cleaning, and the technical solutions of cutting, grinding, polishing and cleaning well known to those skilled in the art can be adopted.
  • the size of the cutting is preferably 12mm ⁇ 12mm ⁇ 12mm; the grinding is preferably polished to 1600# step by step with sandpaper; the polishing material is preferably a polishing cloth; the cleaning is preferably first with acetone Cleaning, and then cleaning with absolute ethanol; the absolute ethanol cleaning is preferably performed under ultrasonic conditions, and the absolute ethanol cleaning time is preferably 15-20 minutes.
  • the applied voltage of the micro-arc oxidation treatment is preferably 380-420V, more preferably 400-420V; the duty cycle is preferably 15-30%, more preferably 20-25%; the frequency is preferably 400- 600Hz, more preferably 550-600Hz; time is preferably 20-25min, more preferably 25min.
  • the voltage of the micro-arc oxidation treatment is too high and the time is too long, the corrosion will be more severe, which will be unfavorable to the strength and corrosion resistance of the alloy.
  • the present invention has no special limitation on the specific operation of the micro-arc oxidation treatment, and the technical solution of the micro-arc oxidation treatment well-known to those skilled in the art can be adopted.
  • the invention forms a ceramic layer on the surface of the AZ80 magnesium alloy through micro-arc oxidation treatment, and the surface of the ceramic layer has a micron-scale porous structure, which is beneficial to improving the corrosion resistance of the alloy.
  • the electrolyte composition of the micro-arc oxidation treatment preferably includes: Na 2 SiO 3 15-20 g/L, NaOH 25-30 g/L, Na 2 B 4 O 7 25-30 g/L and magnetic nickel powder 4g/L, more preferably Na 2 SiO 3 20g/L, NaOH 25g/L, Na 2 B 4 O 7 25g/L and magnetic nickel powder 4g/L.
  • the NaOH is the main component of the electrolyte, and the addition of Na 2 SiO 3 , Na 2 B 4 O 7 and magnetic nickel powder is beneficial to improve the corrosion resistance of the micro-arc oxidation ceramic layer, thereby improving the corrosion resistance of AZ80 magnesium Alloy corrosion resistance.
  • the above-mentioned electrolyte solution is preferably used for micro-arc oxidation treatment.
  • the AZ80 magnesium alloy is used as an anode connected to a micro-arc oxidation power supply, and the cathode is preferably a stainless steel plate.
  • the AZ80 magnesium alloy melt is subjected to spray atomization deposition treatment first, and then homogenization treatment, equal channel angle extrusion deformation and micro-arc oxidation treatment are sequentially performed, and then a strong, tough and corrosion-resistant AZ80 magnesium alloy is obtained. .
  • the invention avoids dendrite segregation and coarse structure of the alloy by adopting atomized deposition treatment, avoids the contact of the alloy with oxygen, and reduces the degree of oxidation of the alloy; by adopting equal channel angle extrusion deformation, the crystal grains can be refined, Improve material toughness, and the ultra-fine grain microstructure formed after equal channel angular extrusion deformation can improve the film formation process of micro-arc oxidation treatment, and improve the compactness of the oxide film on the alloy surface; by adopting micro-arc oxidation treatment on the surface of AZ80 magnesium alloy A ceramic layer is formed, and the surface of the ceramic layer has a micron-scale porous structure, which is beneficial to improving the corrosion resistance of the alloy.
  • the AZ80 magnesium alloy melt was subjected to spray atomization deposition treatment to obtain the deposited AZ80 magnesium alloy billet; wherein, the spray temperature was 760°C, the spray angle was 30°, the atomization medium was high-purity nitrogen, and the atomization pressure was 0.6MPa, the rotating speed of the receiving plate is 50rpm, the descending speed of the receiving plate is 4mm/s, the gas-liquid flow rate ratio is 1.6, the composition of AZ80 magnesium alloy is the following mass percentage content: 7.89% Al, 0.39% Zn, 0.23% Mn , 0.05% Cu, 0.02% Si, 0.01% Fe, and the balance is Mg.
  • step (2) Remove the skin and flash from the deposited AZ80 magnesium alloy billet obtained in step (1), and make a billet with a size of 18mm ⁇ 18mm ⁇ 60mm by wire electric discharge method, and then homogenize it at 390°C After 14 hours, after being polished smooth, place it in an equal-channel angular extrusion deformation mold lubricated by a mixture of graphite powder and kerosene, heat it in the furnace to 230°C and keep it for 20 minutes, and then apply a pressure of 180MPa for 6 consecutive equal-channel angular extrusion deformations.
  • the deformation temperature is 250°C, the deformation speed is 2mm/min; the measured tensile strength at room temperature is 321MPa, the elongation at break is 14%, the full immersion corrosion rate is 4.1mg ⁇ cm -2 h -1 , and the corrosion current density is 133 ⁇ A /cm 2 , the impedance value is 350ohms ⁇ cm 2 .
  • step (3) Cut the AZ80 magnesium alloy after the equal channel angular extrusion deformation treatment in step (2) into a cubic specimen of 12mm ⁇ 12mm ⁇ 12mm, and then polish it step by step with sandpaper to 1600#, polish it with a polishing cloth, and use acetone Clean the surface, ultrasonically clean it in absolute ethanol for 15 minutes, and then put it into the electrolyte.
  • the cubic specimen is used as the anode and connected to the micro-arc oxidation power supply, and the stainless steel plate is connected to the power supply as the cathode.
  • the applied voltage is 420V, and the duty cycle is 25%.
  • the frequency is 600Hz
  • a tough and corrosion-resistant AZ80 magnesium alloy is obtained; among them, the electrolyte composition is: Na 2 SiO 3 20g/L, NaOH 25g/L, Na 2 B 4 O 7 25g/L , magnetic nickel powder 4g/L; the measured tensile strength at room temperature is 321MPa, the elongation at break is 14%, the full immersion corrosion rate is 3.3 ⁇ 10 -4 mg ⁇ cm -2 h -1 , and the corrosion current density is 0.6894 ⁇ A/cm 2 , the impedance value is 7895000ohms ⁇ cm 2 .
  • the AZ80 magnesium alloy melt was subjected to spray atomization deposition treatment to obtain the deposited AZ80 magnesium alloy billet; wherein, the spray temperature was 760°C, the spray angle was 30°, the atomization medium was high-purity nitrogen, and the atomization pressure was 0.6MPa, the rotating speed of the receiving plate is 50rpm, the descending speed of the receiving plate is 4mm/s, the gas-liquid flow rate ratio is 1.6, the composition of AZ80 magnesium alloy is the following mass percentage content: 7.89% Al, 0.39% Zn, 0.23% Mn , 0.05% Cu, 0.02% Si, 0.01% Fe, and the balance is Mg.
  • step (2) Remove the skin and flash from the deposited AZ80 magnesium alloy billet obtained in step (1), and make a billet with a size of 18mm ⁇ 18mm ⁇ 60mm by wire electric discharge method, and then homogenize it at 390°C After 14 hours, after being polished smooth, place it in an equal-channel angular extrusion deformation mold lubricated by a mixture of graphite powder and kerosene, heat it to 230°C for 20 minutes, and then apply a pressure of 180MPa for 10 consecutive equal-channel angular extrusion deformations.
  • the deformation temperature is 250°C, the deformation speed is 2mm/min; the measured tensile strength at room temperature is 334MPa, the tensile elongation at break is 13%, the full immersion corrosion rate is 4.5mg ⁇ cm -2 h -1 , the corrosion current density It is 137 ⁇ A/cm 2 , and the impedance value is 366ohms ⁇ cm 2 .
  • step (3) Cut the AZ80 magnesium alloy after the equal channel angular extrusion deformation treatment in step (2) into a cubic specimen of 12mm ⁇ 12mm ⁇ 12mm, and then polish it step by step with sandpaper to 1600#, polish it with a polishing cloth, and use acetone Clean the surface, ultrasonically clean it in absolute ethanol for 15 minutes, and then put it into the electrolyte.
  • the cubic specimen is used as the anode and connected to the micro-arc oxidation power supply, and the stainless steel plate is connected to the power supply as the cathode.
  • the applied voltage is 420V, and the duty cycle is 25%.
  • the frequency is 600Hz
  • a tough and corrosion-resistant AZ80 magnesium alloy is obtained; among them, the electrolyte composition is: Na 2 SiO 3 20g/L, NaOH 25g/L, Na 2 B 4 O 7 25g/ L, magnetic nickel powder 4g/L; measured tensile strength at room temperature is 334MPa, tensile elongation at break is 13%, full immersion corrosion rate is 3.6 ⁇ 10 -4 mg ⁇ cm -2 h -1 , corrosion current The density is 0.6984 ⁇ A/cm 2 , and the impedance value is 8012000ohms ⁇ cm 2 .
  • the AZ80 magnesium alloy melt was subjected to spray atomization deposition treatment to obtain the deposited AZ80 magnesium alloy billet; wherein, the spray temperature was 760°C, the spray angle was 30°, the atomization medium was high-purity nitrogen, and the atomization pressure was 0.6MPa, the rotating speed of the receiving plate is 50rpm, the descending speed of the receiving plate is 4mm/s, the gas-liquid flow rate ratio is 1.6, the composition of AZ80 magnesium alloy is the following mass percentage content: 7.89% Al, 0.39% Zn, 0.23% Mn , 0.05% Cu, 0.02% Si, 0.01% Fe, and the balance is Mg.
  • step (2) Remove the skin and flash from the deposited AZ80 magnesium alloy billet obtained in step (1), and make a billet with a size of 18mm ⁇ 18mm ⁇ 60mm by wire electric discharge method, and then homogenize it at 390°C After 14 hours, after being polished smooth, place it in an equal-channel angular extrusion deformation mold lubricated by a mixture of graphite powder and kerosene, heat it in the furnace to 230°C and keep it for 20 minutes, and then apply a pressure of 180MPa to carry out 12 consecutive equal-channel angular extrusion deformations.
  • the deformation temperature is 250°C, the deformation speed is 2mm/min; the measured tensile strength at room temperature is 347MPa, the tensile elongation at break is 12.5%, the full immersion corrosion rate is 4.4mg ⁇ cm -2 h -1 , the corrosion current density It is 138 ⁇ A/cm 2 , and the impedance value is 380ohms ⁇ cm 2 .
  • step (3) Cut the AZ80 magnesium alloy after the equal channel angular extrusion deformation treatment in step (2) into a cubic specimen of 12mm ⁇ 12mm ⁇ 12mm, and then polish it step by step with sandpaper to 1600#, polish it with a polishing cloth, and use acetone Clean the surface, ultrasonically clean it in absolute ethanol for 15 minutes, and then put it into the electrolyte.
  • the cubic specimen is used as the anode and connected to the micro-arc oxidation power supply, and the stainless steel plate is connected to the power supply as the cathode.
  • the applied voltage is 400V and the duty cycle is 20%.
  • the frequency is 550Hz
  • a tough and corrosion-resistant AZ80 magnesium alloy is obtained; among them, the electrolyte composition is: Na 2 SiO 3 20g/L, NaOH 25g/L, Na 2 B 4 O 7 25g/ L, magnetic nickel powder 4g/L; measured tensile strength at room temperature is 347MPa, tensile elongation at break is 12.5%, full immersion corrosion rate is 3.5 ⁇ 10 -4 mg ⁇ cm -2 h -1 , corrosion current The density is 0.7041 ⁇ A/cm 2 , and the impedance value is 8082000ohms ⁇ cm 2 .
  • the tough and corrosion-resistant AZ80 magnesium alloy prepared by the preparation method provided by the present invention has good strength and toughness, and excellent corrosion resistance; the room temperature tensile strength of the alloy is 347MPa, and the tensile elongation at break The corrosion rate is 12.5%, the total immersion corrosion rate is 3.5 ⁇ 10 -4 mg ⁇ cm -2 h -1 , the corrosion current density is 0.7041 ⁇ A/cm 2 , and the resistance value is 8082000ohms ⁇ cm 2 .

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Abstract

The present invention relates to the technical field of magnesium alloys, and provides a preparation method for a high-toughness corrosion-resistant AZ80 magnesium alloy, comprising: carrying out jet atomization deposition treatment on an AZ80 magnesium alloy melt, and then sequentially carrying out homogenization treatment, equal channel angular pressing deformation and micro-arc oxidation treatment. According to the present invention, adopting the atomization deposition treatment avoids dendritic segregation and coarse structure of the alloy, and adopting the equal channel angular pressing deformation refines grains, such that the toughness of the material is improved, an ultrafine grain microstructure formed after the equal channel angular pressing deformation can improve the film forming process of micro-arc oxidation treatment, and the compactness of an oxide film on the surface of the alloy is improved. A ceramic layer is formed on the surface of the AZ80 magnesium alloy by using the micro-arc oxidation treatment, such that the corrosion resistance of the alloy is improved. The result of embodiments shows that the tensile strength of the AZ80 magnesium alloy provided by the present invention is 347 MPa, the tensile elongation at break is 12.5%, and the full immersion corrosion rate is 3.5×10-4mg•cm-2h-1.

Description

一种强韧耐蚀AZ80镁合金的制备方法A kind of preparation method of tough and corrosion-resistant AZ80 magnesium alloy 技术领域technical field
本发明涉及镁合金技术领域，尤其涉及一种强韧耐蚀AZ80镁合金的制备方法。The invention relates to the technical field of magnesium alloys, in particular to a preparation method of a strong, tough and corrosion-resistant AZ80 magnesium alloy.
背景技术Background technique
在现有的工程用金属材料中，镁合金作为最轻的金属结构材料之一，被誉为是“21世纪绿色工程材料”，同时镁合金还具有较高的比强度及比刚度、良好的铸造性和尺寸稳定性、高阻尼、电磁干扰屏蔽性能好和回收利用率高等优点，广泛用于航空航天、电子通讯、车辆制造和国防科技等领域。Among the existing metal materials for engineering, magnesium alloy is one of the lightest metal structural materials, and is known as "green engineering material in the 21st century". At the same time, magnesium alloy also has high specific strength and specific stiffness, good With the advantages of castability and dimensional stability, high damping, good electromagnetic interference shielding performance and high recycling rate, it is widely used in aerospace, electronic communication, vehicle manufacturing and national defense technology and other fields.
AZ80镁合金作为镁合金中的一种，表现出了优良的力学性能，然而与钢、铝合金等金属相比，由于镁合金特殊的密排六方的晶格结构，在室温成型时可开动的滑移系非常有限，导致其在室温环境下的韧性较差且强度偏低，很难进行变形加工，进而严重制约了AZ80镁合金的发展，因此开发高性能的AZ80镁合金具有重要意义。As a kind of magnesium alloy, AZ80 magnesium alloy shows excellent mechanical properties. However, compared with steel, aluminum alloy and other metals, due to the special hexagonal close-packed lattice structure of magnesium alloy, it can be activated at room temperature. The slip system is very limited, resulting in poor toughness and low strength at room temperature, making it difficult to deform and process, which severely restricts the development of AZ80 magnesium alloys. Therefore, it is of great significance to develop high-performance AZ80 magnesium alloys.
与此同时，镁的化学性质较为活泼，其标准电极电位为-2.37V，因此即使在自然环境下AZ80镁合金表面生成了氧化膜，也不能够有效的保护金属基体在高温高盐雾等恶劣环境下腐蚀的发生，而这也限制了AZ80镁合金在工业中的应用。At the same time, the chemical properties of magnesium are relatively active, and its standard electrode potential is -2.37V. Therefore, even if an oxide film is formed on the surface of the AZ80 magnesium alloy in the natural environment, it cannot effectively protect the metal substrate from harsh conditions such as high temperature and high salt spray. Corrosion occurs in the environment, which also limits the application of AZ80 magnesium alloy in industry.
发明内容Contents of the invention
本发明的目的在于提供一种强韧耐蚀AZ80镁合金的制备方法，本发明提供的制备方法制备的AZ80镁合金具有良好的强度和韧性，同时耐腐蚀性能优异。The object of the present invention is to provide a method for preparing a strong, tough and corrosion-resistant AZ80 magnesium alloy. The AZ80 magnesium alloy prepared by the preparation method provided by the present invention has good strength and toughness and excellent corrosion resistance.
为了实现上述发明目的，本发明提供了以下技术方案：In order to realize the above-mentioned purpose of the invention, the present invention provides the following technical solutions:
本发明提供了一种强韧耐蚀AZ80镁合金的制备方法，包括以下步骤：The invention provides a preparation method of a tough and corrosion-resistant AZ80 magnesium alloy, comprising the following steps:
(1)将AZ80镁合金熔体进行喷射雾化沉积处理，得到沉积态AZ80镁合金坯锭；(1) AZ80 magnesium alloy melt is subjected to spray atomization deposition treatment to obtain deposited state AZ80 magnesium alloy ingot;
(2)将所述步骤(1)得到的沉积态AZ80镁合金坯锭依次进行均匀化处理、等通道角挤压变形和微弧氧化处理，得到强韧耐蚀AZ80镁合金。(2) The as-deposited AZ80 magnesium alloy ingot obtained in the step (1) is subjected to homogenization treatment, equal channel angular extrusion deformation and micro-arc oxidation treatment sequentially to obtain a strong, tough and corrosion-resistant AZ80 magnesium alloy.
优选地，所述步骤(1)中喷射雾化沉积处理的喷射温度为740～760℃，喷射角度为10～30°。Preferably, the spray temperature of the spray atomization deposition treatment in the step (1) is 740-760° C., and the spray angle is 10-30°.
优选地，所述步骤(1)中喷射雾化沉积处理的雾化压力为0.5～0.7MPa，气液流速比为1.6～1.8。Preferably, the atomization pressure of the spray atomization deposition treatment in the step (1) is 0.5-0.7 MPa, and the gas-liquid flow rate ratio is 1.6-1.8.
优选地，所述步骤(1)中喷射雾化沉积处理的接收盘转速为30～60rpm，接收盘下降速度为2～5mm/s。Preferably, the rotational speed of the receiving tray in the spray atomization deposition treatment in the step (1) is 30-60 rpm, and the descending speed of the receiving tray is 2-5 mm/s.
优选地，所述步骤(2)中均匀化处理的温度为360～400℃，均匀化处理的时间为12～16h。Preferably, the temperature of the homogenization treatment in the step (2) is 360-400° C., and the time of the homogenization treatment is 12-16 hours.
优选地，所述步骤(2)中等通道角挤压变形的温度为250～300℃，速度为2～4mm/min，道次为6、10或12次。Preferably, the temperature of the medium-channel angular extrusion deformation in the step (2) is 250-300° C., the speed is 2-4 mm/min, and the number of passes is 6, 10 or 12.
优选地，所述步骤(2)中等通道角挤压变形的工艺路线为B C，背压力为160～180MPa。 Preferably, the process route of medium channel angular extrusion deformation in the step (2) is B C , and the back pressure is 160-180 MPa.
优选地，所述步骤(2)中微弧氧化处理的外加电压为380～420V，占空比为15～30％，频率为400～600Hz，时间为20～25min。Preferably, the applied voltage of the micro-arc oxidation treatment in the step (2) is 380-420V, the duty ratio is 15-30%, the frequency is 400-600Hz, and the time is 20-25min.
优选地，所述步骤(2)中微弧氧化处理的电解液组成包括：Na 2SiO 315～20g/L，NaOH 25～30g/L，Na 2B 4O 725～30g/L和磁性镍粉体4g/L。 Preferably, the electrolyte composition of the micro-arc oxidation treatment in the step (2) includes: Na 2 SiO 3 15-20g/L, NaOH 25-30g/L, Na 2 B 4 O 7 25-30g/L and magnetic Nickel powder 4g/L.
优选地，所述步骤(1)中AZ80镁合金中包括以下质量百分含量的组分：Al 7.89～8.85％，Zn 0.39～0.50％，Mn 0.23～0.50％，Cu 0.05～0.1％，Si 0.02～0.05％，Fe 0.01～0.03％，余量为Mg。Preferably, the AZ80 magnesium alloy in the step (1) includes the following components in mass percentage: Al 7.89-8.85%, Zn 0.39-0.50%, Mn 0.23-0.50%, Cu 0.05-0.1%, Si 0.02 ～0.05%, Fe 0.01～0.03%, the balance is Mg.
本发明提供了一种强韧耐蚀AZ80镁合金的制备方法，包括以下步骤：将AZ80镁合金熔体进行喷射雾化沉积处理，得到沉积态AZ80镁合金坯锭；将所述沉积态AZ80镁合金坯锭依次进行均匀化处理、等通道角挤压变形和微弧氧化处理，得到强韧耐蚀AZ80镁合金。本发明通过采用雾化沉积处理避免了合金的枝晶偏析和组织粗大，也避免了合金与氧气的接触，减小了合金的氧化程度；通过采用等通道角挤压变形可以细化晶粒，改善材料韧性，并且等通道角挤压变形后形成的超细晶微结构可以改善微弧氧化处理的成膜过程，提高合金表面氧化膜的致密性；通过采用微弧氧化处理在AZ80镁合金表面形成了陶瓷层，且陶瓷层表面呈微米级多孔结构，有利于提高合金的耐蚀性。实施例的结果显示，本发明提供的AZ80镁合金的抗拉强度为347MPa，拉伸断裂伸长率为12.5％，全浸泡腐蚀速率为3.5×10 -4mg·cm -2h -1，腐蚀电流密度为0.7041μA/cm 2，阻抗值为8082000ohms·cm 2。 The invention provides a method for preparing a strong, tough and corrosion-resistant AZ80 magnesium alloy, comprising the following steps: performing spray atomization deposition treatment on an AZ80 magnesium alloy melt to obtain a deposited AZ80 magnesium alloy ingot; The alloy ingot was subjected to homogenization treatment, equal channel angular extrusion deformation and micro-arc oxidation treatment in sequence to obtain a strong, tough and corrosion-resistant AZ80 magnesium alloy. The invention avoids dendrite segregation and coarse structure of the alloy by adopting atomized deposition treatment, avoids the contact of the alloy with oxygen, and reduces the degree of oxidation of the alloy; by adopting equal channel angle extrusion deformation, the crystal grains can be refined, Improve material toughness, and the ultra-fine grain microstructure formed after equal channel angular extrusion deformation can improve the film formation process of micro-arc oxidation treatment, and improve the compactness of the oxide film on the alloy surface; by adopting micro-arc oxidation treatment on the surface of AZ80 magnesium alloy A ceramic layer is formed, and the surface of the ceramic layer has a micron-scale porous structure, which is beneficial to improving the corrosion resistance of the alloy. The results of the examples show that the AZ80 magnesium alloy provided by the present invention has a tensile strength of 347 MPa, a tensile elongation at break of 12.5%, a full immersion corrosion rate of 3.5×10 -4 mg·cm -2 h -1 , and a corrosion rate of The current density is 0.7041 μA/cm 2 , and the impedance value is 8082000 ohms·cm 2 .
具体实施方式detailed description
本发明提供了一种强韧耐蚀AZ80镁合金的制备方法，包括以下步骤：The invention provides a preparation method of a tough and corrosion-resistant AZ80 magnesium alloy, comprising the following steps:
(1)将AZ80镁合金熔体进行喷射雾化沉积处理，得到沉积态AZ80镁合金坯锭；(1) AZ80 magnesium alloy melt is subjected to spray atomization deposition treatment to obtain deposited state AZ80 magnesium alloy ingot;
(2)将所述步骤(1)得到的沉积态AZ80镁合金坯锭依次进行均匀化处理、等通道角挤压变形和微弧氧化处理，得到强韧耐蚀AZ80镁合金。(2) The as-deposited AZ80 magnesium alloy ingot obtained in the step (1) is subjected to homogenization treatment, equal channel angular extrusion deformation and micro-arc oxidation treatment sequentially to obtain a strong, tough and corrosion-resistant AZ80 magnesium alloy.
本发明将AZ80镁合金熔体进行喷射雾化沉积处理，得到沉积态AZ80镁合金坯锭。本发明通过采用雾化沉积处理避免了合金的枝晶偏析和组织粗大，也避免了合金与氧气的接触，减小了合金的氧化程度，有利于提高合金的强度和耐蚀性，且工序简单，成本低，提高了生产效率。In the invention, the AZ80 magnesium alloy melt is subjected to spray atomization deposition treatment to obtain a deposited AZ80 magnesium alloy ingot. The invention avoids dendrite segregation and coarse structure of the alloy by adopting atomization deposition treatment, avoids the contact of the alloy with oxygen, reduces the degree of oxidation of the alloy, is beneficial to improve the strength and corrosion resistance of the alloy, and has a simple process , low cost and improved production efficiency.
本发明对所述AZ80镁合金的组成及来源没有特殊的限定，本发明提供的强韧耐蚀AZ80镁合金的制备方法适用于本领域技术人员熟知的AZ80镁合金。在本发明中，所述AZ80镁合金优选包括以下质量百分含量的组分：Al 7.89～8.85％，Zn 0.39～0.50％，Mn 0.23～0.50％，Cu 0.05～0.1％，Si 0.02～0.05％，Fe 0.01～0.03％，余量为Mg，更优选为Al7.89％，Zn 0.39％，Mn 0.23％，Cu 0.05％，Si 0.02％，Fe 0.01％，余量为Mg。The present invention has no special limitation on the composition and source of the AZ80 magnesium alloy, and the preparation method of the strong and corrosion-resistant AZ80 magnesium alloy provided by the present invention is applicable to the AZ80 magnesium alloy well known to those skilled in the art. In the present invention, the AZ80 magnesium alloy preferably includes the following components in mass percentage: Al 7.89-8.85%, Zn 0.39-0.50%, Mn 0.23-0.50%, Cu 0.05-0.1%, Si 0.02-0.05% , Fe 0.01-0.03%, the balance is Mg, more preferably Al7.89%, Zn 0.39%, Mn 0.23%, Cu 0.05%, Si 0.02%, Fe 0.01%, and the balance is Mg.
在本发明中，所述喷射雾化沉积处理的喷射温度优选为740～760℃，更优选为750～760℃；喷射角度优选为10～30°，更优选为20～30°；雾化介质优选为高纯氮气；雾化压力优选为0.5～0.7MPa，更优选为0.6～0.7MPa；气液流速比优选为1.6～1.8，更优选为1.6；接收盘转速优选为30～60rpm，更优选为50～60rpm；接收盘下降速度优选为2～5mm/s，更优选为4～5mm/s。本发明优选将所述喷射雾化沉积处理的工艺参数控制在上述范围，有利于得到组织均匀的致密化AZ80镁合金坯锭。In the present invention, the spray temperature of the spray atomization deposition treatment is preferably 740-760°C, more preferably 750-760°C; the spray angle is preferably 10-30°, more preferably 20-30°; the atomization medium It is preferably high-purity nitrogen; the atomization pressure is preferably 0.5-0.7MPa, more preferably 0.6-0.7MPa; the gas-liquid flow rate ratio is preferably 1.6-1.8, more preferably 1.6; the speed of the receiving plate is preferably 30-60rpm, more preferably 50-60 rpm; the lowering speed of the receiving tray is preferably 2-5 mm/s, more preferably 4-5 mm/s. In the present invention, the process parameters of the spray atomization deposition treatment are preferably controlled within the above range, which is beneficial to obtain a densified AZ80 magnesium alloy ingot with a uniform structure.
喷射雾化沉积处理完成后，本发明优选去除所述沉积态AZ80镁合金坯锭的表皮和 飞边，并制成尺寸为18mm×18mm×60mm的坯锭。在本发明中，所述坯锭的制备方法优选为电火花线切割法。After the spray atomization deposition treatment is completed, the present invention preferably removes the skin and burrs of the deposited AZ80 magnesium alloy ingot, and makes an ingot with a size of 18mm×18mm×60mm. In the present invention, the method for preparing the ingot is preferably wire electric discharge cutting.
得到沉积态AZ80镁合金坯锭后，本发明将所述沉积态AZ80镁合金坯锭依次进行均匀化处理、等通道角挤压变形和微弧氧化处理，得到强韧耐蚀AZ80镁合金。After the deposited AZ80 magnesium alloy billet is obtained, the invention sequentially performs homogenization treatment, equal channel angular extrusion deformation and micro-arc oxidation treatment on the deposited AZ80 magnesium alloy billet to obtain a strong, tough and corrosion-resistant AZ80 magnesium alloy.
在本发明中，所述均匀化处理的温度优选为360～400℃，更优选为380～390℃；所述均匀化处理的时间优选为12～16h，更优选为14～15h。本发明对所述均匀化处理的具体操作没有特殊的限定，采用本领域技术人员熟知的均匀化处理的技术方案即可。本发明通过均匀化处理使合金铸锭成分均匀化、消除成分偏析和组织不均匀性。In the present invention, the temperature of the homogenization treatment is preferably 360-400° C., more preferably 380-390° C.; the time of the homogenization treatment is preferably 12-16 hours, more preferably 14-15 hours. The present invention has no special limitation on the specific operation of the homogenization treatment, and the technical scheme of homogenization treatment well known to those skilled in the art can be adopted. The invention homogenizes the composition of the alloy ingot through homogenization treatment, and eliminates composition segregation and structure inhomogeneity.
本发明优选将所述均匀化处理后的AZ80镁合金置于润滑剂润滑过的等通道角挤压变形模具中进行保温处理，再进行等通道角挤压变形。在本发明中，所述润滑剂优选包括二硫化钼或石墨粉与煤油的混合物，更优选为石墨粉与煤油的混合物；所述保温处理的温度优选为150～300℃，更优选为230～280℃；保温处理的时间优选为10～20min，更优选为20min。In the present invention, the homogenized AZ80 magnesium alloy is preferably placed in a lubricant-lubricated equal channel angular extrusion deformation mold for heat preservation treatment, and then the equal channel angular extrusion deformation is performed. In the present invention, the lubricant preferably includes molybdenum disulfide or a mixture of graphite powder and kerosene, more preferably a mixture of graphite powder and kerosene; the temperature of the heat preservation treatment is preferably 150-300°C, more preferably 230- 280° C.; the time for heat preservation treatment is preferably 10 to 20 minutes, more preferably 20 minutes.
在本发明中，所述等通道角挤压变形的温度优选为250～300℃，更优选为250～280℃；所述等通道角挤压变形的速度优选为2～4mm/min，更优选为2mm/min。在本发明中，所述等通道角挤压变形的速度过快易出现裂纹，速度过慢浪费能源。在本发明中，所述等通道角挤压变形的道次优选为6、10或12次，更优选为10或12次。本发明优选将所述等通道角挤压变形的道次控制在上述范围，有利于提高组织均匀性。本发明采用等通道角挤压变形可以细化晶粒，改善材料韧性，并且等通道角挤压变形后形成的超细晶微结构可以改善微弧氧化处理的成膜过程，提高合金表面氧化膜的致密性，进而提高了AZ80镁合金的耐蚀性能。In the present invention, the temperature of the equal channel angular extrusion deformation is preferably 250-300°C, more preferably 250-280°C; the speed of the equal channel angular extrusion deformation is preferably 2-4mm/min, more preferably It is 2mm/min. In the present invention, if the deformation speed of the equal channel angular extrusion is too fast, cracks will easily appear, and if the speed is too slow, energy will be wasted. In the present invention, the number of passes of the equal channel angular extrusion deformation is preferably 6, 10 or 12 times, more preferably 10 or 12 times. In the present invention, the number of passes of the equal channel angular extrusion deformation is preferably controlled within the above range, which is beneficial to improving the uniformity of the tissue. The present invention adopts equal channel angular extrusion deformation to refine crystal grains and improve material toughness, and the ultra-fine grain microstructure formed after equal channel angular extrusion deformation can improve the film forming process of micro-arc oxidation treatment and improve the oxidation film on the surface of the alloy. The compactness, thereby improving the corrosion resistance of AZ80 magnesium alloy.
在本发明中，所述等通道角挤压变形的工艺路线优选为B C；本发明采用Bc工艺路线，相邻挤压道次之间样品旋转90°，有利于提高组织均匀性。在本发明中，所述等通道角挤压变形的背压力优选为160～180MPa，更优选为170～180MPa。在本发明中，所述等通道角挤压变形的背压力用于调节模具里的压力平衡，将其控制在上述范围，有利于使塑性变形更稳定。 In the present invention, the process route of the equal channel angular extrusion deformation is preferably B C ; the present invention adopts the Bc process route, and the sample is rotated by 90° between adjacent extrusion passes, which is beneficial to improve the uniformity of the structure. In the present invention, the back pressure of the equal channel angular extrusion deformation is preferably 160-180 MPa, more preferably 170-180 MPa. In the present invention, the back pressure of the equal channel angular extrusion deformation is used to adjust the pressure balance in the mold, and controlling it within the above range is beneficial to make the plastic deformation more stable.
本发明优选将所述等通道角挤压变形后的AZ80镁合金依次进行切割、打磨、抛光和清洗，再进行微弧氧化处理。本发明对所述切割、打磨、抛光和清洗的操作没有特殊的限定，采用本领域技术人员熟知的切割、打磨、抛光和清洗的技术方案即可。在本发明中，所述切割的尺寸优选为12mm×12mm×12mm；所述打磨优选为用砂纸逐级打磨至1600#；所述抛光的材料优选为抛光布；所述清洗优选为先用丙酮清洗，再用无水乙醇清洗；所述无水乙醇清洗优选在超声的条件下进行，所述无水乙醇清洗的时间优选为15～20min。In the present invention, the AZ80 magnesium alloy deformed by equal channel angular extrusion is preferably cut, polished, polished and cleaned in sequence, and then subjected to micro-arc oxidation treatment. The present invention has no special limitation on the operations of cutting, grinding, polishing and cleaning, and the technical solutions of cutting, grinding, polishing and cleaning well known to those skilled in the art can be adopted. In the present invention, the size of the cutting is preferably 12mm × 12mm × 12mm; the grinding is preferably polished to 1600# step by step with sandpaper; the polishing material is preferably a polishing cloth; the cleaning is preferably first with acetone Cleaning, and then cleaning with absolute ethanol; the absolute ethanol cleaning is preferably performed under ultrasonic conditions, and the absolute ethanol cleaning time is preferably 15-20 minutes.
在本发明中，所述微弧氧化处理的外加电压优选为380～420V，更优选为400～420V；占空比优选为15～30％，更优选为20～25％；频率优选为400～600Hz，更优选为550～600Hz；时间优选为20～25min，更优选为25min。在本发明中，所述微弧氧化处理的电压过高、时间过久，腐蚀越厉害，对合金的强度和耐蚀性能不利。本发明对所述微弧氧化处理的具体操作没有特殊的限定，采用本领域技术人员熟知的微弧氧化处理的技术方案即可。本发明通过采用微弧氧化处理在AZ80镁合金表面形成了陶瓷层，且陶瓷层表面呈微米级多孔结构，有利于提高合金的耐蚀性。In the present invention, the applied voltage of the micro-arc oxidation treatment is preferably 380-420V, more preferably 400-420V; the duty cycle is preferably 15-30%, more preferably 20-25%; the frequency is preferably 400- 600Hz, more preferably 550-600Hz; time is preferably 20-25min, more preferably 25min. In the present invention, if the voltage of the micro-arc oxidation treatment is too high and the time is too long, the corrosion will be more severe, which will be unfavorable to the strength and corrosion resistance of the alloy. The present invention has no special limitation on the specific operation of the micro-arc oxidation treatment, and the technical solution of the micro-arc oxidation treatment well-known to those skilled in the art can be adopted. The invention forms a ceramic layer on the surface of the AZ80 magnesium alloy through micro-arc oxidation treatment, and the surface of the ceramic layer has a micron-scale porous structure, which is beneficial to improving the corrosion resistance of the alloy.
在本发明中，所述微弧氧化处理的电解液组成优选包括：Na 2SiO 3 15～20g/L，NaOH 25～30g/L，Na 2B 4O 7 25～30g/L和磁性镍粉体4g/L，更优选为Na 2SiO 3 20g/L，NaOH 25g/L，Na 2B 4O 7 25g/L和磁性镍粉体4g/L。在本发明中，所述NaOH为电解液的主要成分，Na 2SiO 3、Na 2B 4O 7和磁性镍粉体的添加有利于提高微弧氧化陶瓷层的耐蚀性能，进而提高AZ80镁合金的耐蚀性能。本发明优选采用上述电解液用于微弧氧化处理，腐蚀液浓度越大，腐蚀越厉害，容易出现沿晶界断裂。在本发明中，所述AZ80镁合金作为阳极与微弧氧化电源相连，所述阴极优选为不锈钢板。 In the present invention, the electrolyte composition of the micro-arc oxidation treatment preferably includes: Na 2 SiO 3 15-20 g/L, NaOH 25-30 g/L, Na 2 B 4 O 7 25-30 g/L and magnetic nickel powder 4g/L, more preferably Na 2 SiO 3 20g/L, NaOH 25g/L, Na 2 B 4 O 7 25g/L and magnetic nickel powder 4g/L. In the present invention, the NaOH is the main component of the electrolyte, and the addition of Na 2 SiO 3 , Na 2 B 4 O 7 and magnetic nickel powder is beneficial to improve the corrosion resistance of the micro-arc oxidation ceramic layer, thereby improving the corrosion resistance of AZ80 magnesium Alloy corrosion resistance. In the present invention, the above-mentioned electrolyte solution is preferably used for micro-arc oxidation treatment. The greater the concentration of the corrosive solution, the more severe the corrosion, and the fracture along the grain boundary is prone to occur. In the present invention, the AZ80 magnesium alloy is used as an anode connected to a micro-arc oxidation power supply, and the cathode is preferably a stainless steel plate.
本发明提供的制备方法通过先将AZ80镁合金熔体进行喷射雾化沉积处理，再依次进行均匀化处理、等通道角挤压变形和微弧氧化处理，进而得到了强韧耐蚀AZ80镁合金。本发明通过采用雾化沉积处理避免了合金的枝晶偏析和组织粗大，也避免了合金与氧气的接触，减小了合金的氧化程度；通过采用等通道角挤压变形可以细化晶粒，改善材料韧性，并且等通道角挤压变形后形成的超细晶微结构可以改善微弧氧化处理的成膜过程，提高合金表面氧化膜的致密性；通过采用微弧氧化处理在AZ80镁合金表面形成了陶瓷层，且陶瓷层表面呈微米级多孔结构，有利于提高合金的耐蚀性。In the preparation method provided by the present invention, the AZ80 magnesium alloy melt is subjected to spray atomization deposition treatment first, and then homogenization treatment, equal channel angle extrusion deformation and micro-arc oxidation treatment are sequentially performed, and then a strong, tough and corrosion-resistant AZ80 magnesium alloy is obtained. . The invention avoids dendrite segregation and coarse structure of the alloy by adopting atomized deposition treatment, avoids the contact of the alloy with oxygen, and reduces the degree of oxidation of the alloy; by adopting equal channel angle extrusion deformation, the crystal grains can be refined, Improve material toughness, and the ultra-fine grain microstructure formed after equal channel angular extrusion deformation can improve the film formation process of micro-arc oxidation treatment, and improve the compactness of the oxide film on the alloy surface; by adopting micro-arc oxidation treatment on the surface of AZ80 magnesium alloy A ceramic layer is formed, and the surface of the ceramic layer has a micron-scale porous structure, which is beneficial to improving the corrosion resistance of the alloy.
下面将结合本发明中的实施例，对本发明中的技术方案进行清楚、完整地描述。显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solutions in the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Apparently, the described embodiments are only some of the embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
实施例1Example 1
(1)将AZ80镁合金熔体进行喷射雾化沉积处理，得到沉积态AZ80镁合金坯锭；其中，喷射温度为760℃，喷射角度为30°，雾化介质为高纯氮气，雾化压力为0.6MPa，接收盘转速为50rpm，接收盘下降速度为4mm/s，气液流速比为1.6，AZ80镁合金的组分为以下质量百分含量：7.89％Al，0.39％Zn，0.23％Mn，0.05％Cu，0.02％Si，0.01％Fe，余量为Mg。(1) The AZ80 magnesium alloy melt was subjected to spray atomization deposition treatment to obtain the deposited AZ80 magnesium alloy billet; wherein, the spray temperature was 760°C, the spray angle was 30°, the atomization medium was high-purity nitrogen, and the atomization pressure was 0.6MPa, the rotating speed of the receiving plate is 50rpm, the descending speed of the receiving plate is 4mm/s, the gas-liquid flow rate ratio is 1.6, the composition of AZ80 magnesium alloy is the following mass percentage content: 7.89% Al, 0.39% Zn, 0.23% Mn , 0.05% Cu, 0.02% Si, 0.01% Fe, and the balance is Mg.
(2)将步骤(1)得到的沉积态AZ80镁合金坯锭去除表皮和飞边，并通过电火花线切割法制成尺寸为18mm×18mm×60mm的坯锭，之后在390℃下均匀化处理14h，打磨光滑后置于经石墨粉与煤油的混合物润滑过的等通道角挤压变形模具中随炉加热至230℃保温20min，再施加180MPa压力进行连续6道次等通道角挤压变形，变形温度为250℃，变形速度为2mm/min；测得室温抗拉强度为321MPa，断裂伸长率为14％，全浸泡腐蚀速率为4.1mg·cm -2h -1，腐蚀电流密度为133μA/cm 2，阻抗值为350ohms·cm 2。 (2) Remove the skin and flash from the deposited AZ80 magnesium alloy billet obtained in step (1), and make a billet with a size of 18mm×18mm×60mm by wire electric discharge method, and then homogenize it at 390°C After 14 hours, after being polished smooth, place it in an equal-channel angular extrusion deformation mold lubricated by a mixture of graphite powder and kerosene, heat it in the furnace to 230°C and keep it for 20 minutes, and then apply a pressure of 180MPa for 6 consecutive equal-channel angular extrusion deformations. The deformation temperature is 250℃, the deformation speed is 2mm/min; the measured tensile strength at room temperature is 321MPa, the elongation at break is 14%, the full immersion corrosion rate is 4.1mg·cm -2 h -1 , and the corrosion current density is 133μA /cm 2 , the impedance value is 350ohms·cm 2 .
(3)将步骤(2)经过等通道角挤压变形处理后的AZ80镁合金切割成12mm×12mm×12mm的立方试件，再用砂纸逐级打磨至1600#、抛光布抛光，用丙酮进行表面清洗，并在无水乙醇中超声波清洗15min后放入电解液中，立方试件作为阳极与微弧氧化电源相连，不锈钢板与电源相连作为阴极，外加电压为420V，占空比为25％，频率为600Hz，微弧氧化处理25min后，得到强韧耐蚀AZ80镁合金；其中，电解液组成为：Na 2SiO 3 20g/L，NaOH 25g/L，Na 2B 4O 7 25g/L，磁性镍粉体4g/L；测得室温抗拉强度为321MPa，断裂伸长率为14％，全浸泡腐蚀速率为3.3×10 -4mg·cm -2h -1，腐蚀电流密度为0.6894μA/cm 2，阻抗值为7895000ohms·cm 2。 (3) Cut the AZ80 magnesium alloy after the equal channel angular extrusion deformation treatment in step (2) into a cubic specimen of 12mm×12mm×12mm, and then polish it step by step with sandpaper to 1600#, polish it with a polishing cloth, and use acetone Clean the surface, ultrasonically clean it in absolute ethanol for 15 minutes, and then put it into the electrolyte. The cubic specimen is used as the anode and connected to the micro-arc oxidation power supply, and the stainless steel plate is connected to the power supply as the cathode. The applied voltage is 420V, and the duty cycle is 25%. , the frequency is 600Hz, and after micro-arc oxidation treatment for 25 minutes, a tough and corrosion-resistant AZ80 magnesium alloy is obtained; among them, the electrolyte composition is: Na 2 SiO 3 20g/L, NaOH 25g/L, Na 2 B 4 O 7 25g/L , magnetic nickel powder 4g/L; the measured tensile strength at room temperature is 321MPa, the elongation at break is 14%, the full immersion corrosion rate is 3.3×10 -4 mg·cm -2 h -1 , and the corrosion current density is 0.6894 μA/cm 2 , the impedance value is 7895000ohms·cm 2 .
实施例2Example 2
(1)将AZ80镁合金熔体进行喷射雾化沉积处理，得到沉积态AZ80镁合金坯锭；其 中，喷射温度为760℃，喷射角度为30°，雾化介质为高纯氮气，雾化压力为0.6MPa，接收盘转速为50rpm，接收盘下降速度为4mm/s，气液流速比为1.6，AZ80镁合金的组分为以下质量百分含量：7.89％Al，0.39％Zn，0.23％Mn，0.05％Cu，0.02％Si，0.01％Fe，余量为Mg。(1) The AZ80 magnesium alloy melt was subjected to spray atomization deposition treatment to obtain the deposited AZ80 magnesium alloy billet; wherein, the spray temperature was 760°C, the spray angle was 30°, the atomization medium was high-purity nitrogen, and the atomization pressure was 0.6MPa, the rotating speed of the receiving plate is 50rpm, the descending speed of the receiving plate is 4mm/s, the gas-liquid flow rate ratio is 1.6, the composition of AZ80 magnesium alloy is the following mass percentage content: 7.89% Al, 0.39% Zn, 0.23% Mn , 0.05% Cu, 0.02% Si, 0.01% Fe, and the balance is Mg.
(2)将步骤(1)得到的沉积态AZ80镁合金坯锭去除表皮和飞边，并通过电火花线切割法制成尺寸为18mm×18mm×60mm的坯锭，之后在390℃下均匀化处理14h，打磨光滑后置于经石墨粉与煤油的混合物润滑过的等通道角挤压变形模具中随炉加热至230℃保温20min，再施加180MPa压力进行连续10道次等通道角挤压变形，变形温度为250℃，变形速度为2mm/min；测得室温抗拉强度为334MPa，拉伸断裂伸长率为13％，全浸泡腐蚀速率为4.5mg·cm -2h -1，腐蚀电流密度为137μA/cm 2，阻抗值为366ohms·cm 2。 (2) Remove the skin and flash from the deposited AZ80 magnesium alloy billet obtained in step (1), and make a billet with a size of 18mm×18mm×60mm by wire electric discharge method, and then homogenize it at 390°C After 14 hours, after being polished smooth, place it in an equal-channel angular extrusion deformation mold lubricated by a mixture of graphite powder and kerosene, heat it to 230°C for 20 minutes, and then apply a pressure of 180MPa for 10 consecutive equal-channel angular extrusion deformations. The deformation temperature is 250℃, the deformation speed is 2mm/min; the measured tensile strength at room temperature is 334MPa, the tensile elongation at break is 13%, the full immersion corrosion rate is 4.5mg·cm -2 h -1 , the corrosion current density It is 137μA/cm 2 , and the impedance value is 366ohms·cm 2 .
(3)将步骤(2)经过等通道角挤压变形处理后的AZ80镁合金切割成12mm×12mm×12mm的立方试件，再用砂纸逐级打磨至1600#、抛光布抛光，用丙酮进行表面清洗，并在无水乙醇中超声波清洗15min后放入电解液中，立方试件作为阳极与微弧氧化电源相连，不锈钢板与电源相连作为阴极，外加电压为420V，占空比为25％，频率为600Hz，微弧氧化处理25min后，制得强韧耐蚀AZ80镁合金；其中，电解液组成为：Na 2SiO 3 20g/L，NaOH 25g/L，Na 2B 4O 7 25g/L，磁性镍粉体4g/L；测得室温抗拉强度为334MPa，拉伸断裂伸长率为13％，全浸泡腐蚀速率为3.6×10 -4mg·cm -2h -1，腐蚀电流密度为0.6984μA/cm 2，阻抗值为8012000ohms·cm 2。 (3) Cut the AZ80 magnesium alloy after the equal channel angular extrusion deformation treatment in step (2) into a cubic specimen of 12mm×12mm×12mm, and then polish it step by step with sandpaper to 1600#, polish it with a polishing cloth, and use acetone Clean the surface, ultrasonically clean it in absolute ethanol for 15 minutes, and then put it into the electrolyte. The cubic specimen is used as the anode and connected to the micro-arc oxidation power supply, and the stainless steel plate is connected to the power supply as the cathode. The applied voltage is 420V, and the duty cycle is 25%. , the frequency is 600Hz, and after micro-arc oxidation treatment for 25min, a tough and corrosion-resistant AZ80 magnesium alloy is obtained; among them, the electrolyte composition is: Na 2 SiO 3 20g/L, NaOH 25g/L, Na 2 B 4 O 7 25g/ L, magnetic nickel powder 4g/L; measured tensile strength at room temperature is 334MPa, tensile elongation at break is 13%, full immersion corrosion rate is 3.6×10 -4 mg·cm -2 h -1 , corrosion current The density is 0.6984μA/cm 2 , and the impedance value is 8012000ohms·cm 2 .
实施例3Example 3
(1)将AZ80镁合金熔体进行喷射雾化沉积处理，得到沉积态AZ80镁合金坯锭；其中，喷射温度为760℃，喷射角度为30°，雾化介质为高纯氮气，雾化压力为0.6MPa，接收盘转速为50rpm，接收盘下降速度为4mm/s，气液流速比为1.6，AZ80镁合金的组分为以下质量百分含量：7.89％Al，0.39％Zn，0.23％Mn，0.05％Cu，0.02％Si，0.01％Fe，余量为Mg。(1) The AZ80 magnesium alloy melt was subjected to spray atomization deposition treatment to obtain the deposited AZ80 magnesium alloy billet; wherein, the spray temperature was 760°C, the spray angle was 30°, the atomization medium was high-purity nitrogen, and the atomization pressure was 0.6MPa, the rotating speed of the receiving plate is 50rpm, the descending speed of the receiving plate is 4mm/s, the gas-liquid flow rate ratio is 1.6, the composition of AZ80 magnesium alloy is the following mass percentage content: 7.89% Al, 0.39% Zn, 0.23% Mn , 0.05% Cu, 0.02% Si, 0.01% Fe, and the balance is Mg.
(2)将步骤(1)得到的沉积态AZ80镁合金坯锭去除表皮和飞边，并通过电火花线切割法制成尺寸为18mm×18mm×60mm的坯锭，之后在390℃下均匀化处理14h，打磨光滑后置于经石墨粉与煤油的混合物润滑过的等通道角挤压变形模具中随炉加热至230℃保温20min，再施加180MPa压力进行连续12道次等通道角挤压变形，变形温度为250℃，变形速度为2mm/min；测得室温抗拉强度为347MPa，拉伸断裂伸长率为12.5％，全浸泡腐蚀速率为4.4mg·cm -2h -1，腐蚀电流密度为138μA/cm 2，阻抗值为380ohms·cm 2。 (2) Remove the skin and flash from the deposited AZ80 magnesium alloy billet obtained in step (1), and make a billet with a size of 18mm×18mm×60mm by wire electric discharge method, and then homogenize it at 390°C After 14 hours, after being polished smooth, place it in an equal-channel angular extrusion deformation mold lubricated by a mixture of graphite powder and kerosene, heat it in the furnace to 230°C and keep it for 20 minutes, and then apply a pressure of 180MPa to carry out 12 consecutive equal-channel angular extrusion deformations. The deformation temperature is 250℃, the deformation speed is 2mm/min; the measured tensile strength at room temperature is 347MPa, the tensile elongation at break is 12.5%, the full immersion corrosion rate is 4.4mg·cm -2 h -1 , the corrosion current density It is 138μA/cm 2 , and the impedance value is 380ohms·cm 2 .
(3)将步骤(2)经过等通道角挤压变形处理后的AZ80镁合金切割成12mm×12mm×12mm的立方试件，再用砂纸逐级打磨至1600#、抛光布抛光，用丙酮进行表面清洗，并在无水乙醇中超声波清洗15min后放入电解液中，立方试件作为阳极与微弧氧化电源相连，不锈钢板与电源相连作为阴极，外加电压为400V，占空比为20％，频率为550Hz，微弧氧化处理25min后，制得强韧耐蚀AZ80镁合金；其中，电解液组成为：Na 2SiO 3 20g/L，NaOH 25g/L，Na 2B 4O 7 25g/L，磁性镍粉体4g/L；测得室温抗拉强度为347MPa，拉伸断裂伸长率为12.5％，全浸泡腐蚀速率为3.5×10 -4mg·cm -2h -1，腐蚀电流密度为0.7041μA/cm 2，阻抗值为8082000ohms·cm 2。 (3) Cut the AZ80 magnesium alloy after the equal channel angular extrusion deformation treatment in step (2) into a cubic specimen of 12mm×12mm×12mm, and then polish it step by step with sandpaper to 1600#, polish it with a polishing cloth, and use acetone Clean the surface, ultrasonically clean it in absolute ethanol for 15 minutes, and then put it into the electrolyte. The cubic specimen is used as the anode and connected to the micro-arc oxidation power supply, and the stainless steel plate is connected to the power supply as the cathode. The applied voltage is 400V and the duty cycle is 20%. , the frequency is 550Hz, and after micro-arc oxidation treatment for 25min, a tough and corrosion-resistant AZ80 magnesium alloy is obtained; among them, the electrolyte composition is: Na 2 SiO 3 20g/L, NaOH 25g/L, Na 2 B 4 O 7 25g/ L, magnetic nickel powder 4g/L; measured tensile strength at room temperature is 347MPa, tensile elongation at break is 12.5%, full immersion corrosion rate is 3.5×10 -4 mg·cm -2 h -1 , corrosion current The density is 0.7041μA/cm 2 , and the impedance value is 8082000ohms·cm 2 .
由以上实施例可以看出，本发明提供的制备方法制备的强韧耐蚀AZ80镁合金具有良好的强度和韧性，同时耐腐蚀性能优异；合金的室温抗拉强度为347MPa，拉伸断裂伸长率为12.5％，全浸泡腐蚀速率为3.5×10 -4mg·cm -2h -1，腐蚀电流密度为0.7041μA/cm 2，阻抗值 为8082000ohms·cm 2。 As can be seen from the above examples, the tough and corrosion-resistant AZ80 magnesium alloy prepared by the preparation method provided by the present invention has good strength and toughness, and excellent corrosion resistance; the room temperature tensile strength of the alloy is 347MPa, and the tensile elongation at break The corrosion rate is 12.5%, the total immersion corrosion rate is 3.5×10 -4 mg·cm -2 h -1 , the corrosion current density is 0.7041μA/cm 2 , and the resistance value is 8082000ohms·cm 2 .
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, it should be pointed out that, for those of ordinary skill in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications can also be made. It should be regarded as the protection scope of the present invention.

Claims (4)

  1. 一种强韧耐蚀AZ80镁合金的制备方法，包括以下步骤：A preparation method for a tough and corrosion-resistant AZ80 magnesium alloy, comprising the following steps:
    (1)将AZ80镁合金熔体进行喷射雾化沉积处理，得到沉积态AZ80镁合金坯锭；所述喷射雾化沉积处理的喷射温度为740～760℃，喷射角度为10～30°，雾化压力为0.5～0.7MPa，气液流速比为1.6～1.8，接收盘转速为30～60rpm，接收盘下降速度为2～5mm/s；(1) AZ80 magnesium alloy melt is subjected to spray atomization deposition treatment to obtain deposited state AZ80 magnesium alloy ingot; the spray temperature of the spray atomization deposition treatment is 740-760°C, the spray angle is 10-30°, and the spray The melting pressure is 0.5-0.7MPa, the gas-liquid flow rate ratio is 1.6-1.8, the rotating speed of the receiving plate is 30-60rpm, and the falling speed of the receiving plate is 2-5mm/s;
    所述AZ80镁合金由以下质量百分含量的组分组成：Al 7.89～8.85％，Zn 0.39～0.50％，Mn 0.23～0.50％，Cu 0.05～0.1％，Si 0.02～0.05％，Fe 0.01～0.03％，余量为Mg；The AZ80 magnesium alloy is composed of the following components in mass percentage: Al 7.89-8.85%, Zn 0.39-0.50%, Mn 0.23-0.50%, Cu 0.05-0.1%, Si 0.02-0.05%, Fe 0.01-0.03 %, the balance is Mg;
    (2)将所述步骤(1)得到的沉积态AZ80镁合金坯锭依次进行均匀化处理、等通道角挤压变形和微弧氧化处理，得到强韧耐蚀AZ80镁合金；所述均匀化处理的温度为360～400℃，均匀化处理的时间为12～16h；所述等通道角挤压变形的温度为250～300℃，速度为2～4mm/min，道次为6、10或12次。(2) The deposition state AZ80 magnesium alloy ingot obtained in the step (1) is subjected to homogenization treatment, equal channel angular extrusion deformation and micro-arc oxidation treatment successively to obtain a tough and corrosion-resistant AZ80 magnesium alloy; the homogenization The temperature of the treatment is 360-400°C, and the homogenization treatment time is 12-16h; the temperature of the equal channel angular extrusion deformation is 250-300°C, the speed is 2-4mm/min, and the number of passes is 6, 10 or 12 times.
  2. 根据权利要求1所述的制备方法，其特征在于，所述步骤(2)中等通道角挤压变形的工艺路线为B C，背压力为160～180MPa。 The preparation method according to claim 1, characterized in that, the process route of medium channel angular extrusion deformation in the step (2) is B C , and the back pressure is 160-180 MPa.
  3. 根据权利要求1所述的制备方法，其特征在于，所述步骤(2)中微弧氧化处理的外加电压为380～420V，占空比为15～30％，频率为400～600Hz，时间为20～25min。The preparation method according to claim 1, characterized in that the applied voltage of the micro-arc oxidation treatment in the step (2) is 380-420V, the duty cycle is 15-30%, the frequency is 400-600Hz, and the time is 20～25min.
  4. 根据权利要求1或3所述的制备方法，其特征在于，所述步骤(2)中微弧氧化处理的电解液组成包括：Na 2SiO 3 15～20g/L，NaOH 25～30g/L，Na 2B 4O 7 25～30g/L和磁性镍粉体4g/L。 The preparation method according to claim 1 or 3, characterized in that the electrolyte composition of the micro-arc oxidation treatment in the step (2) includes: Na 2 SiO 3 15-20g/L, NaOH 25-30g/L, Na 2 B 4 O 7 25～30g/L and magnetic nickel powder 4g/L.
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