CN109666877B - High-temperature treatment method for aluminum alloy with low-melting-point eutectic structure - Google Patents
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- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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Abstract
The invention discloses a high-temperature treatment method of an aluminum alloy with a low-melting-point eutectic structure, which comprises the steps of firstly determining the low-melting-point eutectic temperature and the melting point of an aluminum alloy ingot to be treated through differential scanning calorimetry analysis; putting the aluminum alloy cast ingot into a heat treatment furnace, heating the aluminum alloy cast ingot from room temperature to a temperature above the eutectic temperature with a low melting point and below the melting point, then preserving the heat for 4-8 hours, taking out and quenching; the aluminum alloy cast ingot comprises the following components in percentage by mass: zn is less than or equal to 5, In is less than or equal to 0.03, Er is 0.6-4, and the balance is Al. Compared with common heat treatment, the high temperature treatment method of the aluminum alloy can homogenize segregation structure and precipitate proper amount of spheroidized structure.
Description
Technical Field
The invention relates to the technical field of heat treatment of aluminum alloy materials, in particular to a high-temperature treatment method of an aluminum alloy with a low-melting-point eutectic structure.
Background
The purpose of the high-temperature homogenization heat treatment of the aluminum alloy is to improve the mechanical property and the electrochemical property of the aluminum alloy as an anode material, a eutectic structure with a low melting point can be obtained by DSC analysis, and the DSC analysis curve of the Al-Zn-In-Er alloy is shown as figure 1 and is 610 ℃ and the melting point is 638.5 ℃.
The research of the Al-Zn-In anode material shows that the intergranular segregation is not improved, the intergranular segregation phenomenon of the Al-Zn-In-Er alloy is serious when the temperature is further increased, the existence of a segregation phase influences the mechanical property of the alloy, and the potential difference between a crystal boundary and a matrix is caused, so that the galvanic corrosion is caused when the alloy is used as the anode material. The grain boundary segregation of the alloy can be improved to different degrees through homogenization, and the grain boundary segregation phenomenon in the alloy structure is not fundamentally improved when the common homogenization treatment is carried out at the homogenization temperature of 535 ℃ of the common Al-Zn series alloy. The Al-Zn-In-Er alloy is further heated to above 610 ℃, the grain boundary segregation phase In the alloy structure is greatly reduced, the matrix is accompanied with the precipitation of a spheroidized structure, and at the moment, the alloy does not have other overburning characteristics. The research shows that the structure is a low-melting-point eutectic structure of the alloy, and is a eutectic structure of a compound of rare earth elements and aluminum, an alpha phase and an In phase, and the research finds that the alloy is subjected to high-temperature treatment by being higher than the melting point of the low-melting-point eutectic structure, and the alloy has a proper amount of low-melting-point eutectic structure after being cooled, so that the hardness of the alloy is improved, and the alloy can be used as an anode material.
Disclosure of Invention
The invention aims to: in view of the above problems, a high-temperature treatment method for an aluminum alloy having a low-melting eutectic structure is provided.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a high-temperature treatment method of an aluminum alloy with a low-melting-point eutectic structure comprises the following steps:
(1) firstly, determining the low-melting-point eutectic temperature and the melting point of the aluminum alloy cast ingot to be treated through differential scanning calorimetry analysis;
(2) putting the aluminum alloy cast ingot into a heat treatment furnace, heating the aluminum alloy cast ingot from room temperature to a temperature above the eutectic temperature with a low melting point and below the melting point, then preserving the heat for 4-8 hours, taking out and quenching;
the aluminum alloy cast ingot comprises the following components in percentage by mass: zn is less than or equal to 5, In is less than or equal to 0.03, Er is 0.6-4, and the balance is Al.
Preferably, the temperature is raised to 0-20 ℃ above the eutectic temperature with low melting point, and then the temperature is kept.
Preferably, the temperature rise speed is 2-10 ℃/min.
Preferably, when the temperature of the aluminum alloy ingot is lower than 580 ℃, the heating rate is 5-10 ℃/min; when the temperature of the aluminum alloy cast ingot is higher than 580 ℃, the heating rate is 2-5 ℃/min.
Preferably, the preparation method of the aluminum alloy ingot comprises the following steps:
(1) putting an aluminum ingot into the crucible, and then heating; when the temperature is raised to 750-;
(2) keeping the temperature unchanged, and adding the Al-Zn intermediate alloy after the Al-Er intermediate alloy is completely melted;
(3) keeping the temperature unchanged, adding a refining agent after the Al-Zn intermediate alloy is completely melted, fully stirring, and then standing for 10-15 min; the purpose is to remove gas in the melt, purify the melt,
(4) keeping the temperature unchanged, adding the Al-In intermediate alloy, and casting after the Al-In intermediate alloy is completely melted.
Preferably, before the aluminum ingot is put into the crucible, a proper amount of pure aluminum is put into the crucible, the temperature is raised to 750 ℃, the whole crucible is poured by a spoon after the pure aluminum is fully melted, and then the crucible is kept stand for 15-30min and poured out. The purpose is to clean the crucible with molten pure metal to remove other impurities.
Preferably, the casting is carried out at a temperature of 740 ℃ and 760 ℃.
Preferably, the refining agent is C2Cl6The addition amount of the refining agent is 0.5-2% of the total weight of the alloy in the crucible.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
compared with common heat treatment, the high temperature treatment method of the aluminum alloy can homogenize segregation structure and precipitate proper amount of spheroidized structure.
Drawings
FIG. 1 is a DSC analysis of an as-cast alloy;
FIG. 2 is a structural diagram of the alloy before and after heat treatment, (a) before heat treatment and (b) after heat treatment;
FIG. 3 shows the results of polarization curves of the alloy before and after heat treatment.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to preferred embodiments. It should be noted, however, that the numerous details set forth in the description are merely for the purpose of providing the reader with a thorough understanding of one or more aspects of the present invention, which may be practiced without these specific details.
Example 1
A high-temperature treatment method of an aluminum alloy with a low-melting-point eutectic structure comprises the following steps:
step 1: alloy smelting: the aluminum alloy cast ingot comprises the following components in percentage by weight: the zinc content is 5% in addition to the aluminum; the indium content is 0.03%; the erbium content was 1%.
(1) Putting a proper amount of pure aluminum into the crucible for cleaning and preheating the crucible, heating the crucible to 750 ℃, pouring the whole crucible by using an iron ladle coated with a protective coating after the pure aluminum is fully melted, standing for 15min, and pouring out; (2) putting all aluminum ingots into the crucible, and then heating;after the temperature is raised to 780 ℃, putting Al-Er intermediate alloy after the aluminum ingot is completely melted; (3) keeping the temperature unchanged, and adding the Al-Zn intermediate alloy after the Al-Er intermediate alloy is completely melted; (4) keeping the temperature unchanged, adding C accounting for 0.5 percent of the total weight of the alloy in the crucible after the Al-Zn intermediate alloy is completely melted2Cl6Refining, stirring thoroughly, standing for 10min, and removing slag with an iron ladle coated with a protective coating; keeping the temperature unchanged, and adding Al-In intermediate alloy; pouring the melt at 750 ℃ to obtain an aluminum alloy ingot;
step 2: high-temperature treatment: firstly, determining the low-melting-point eutectic temperature and the melting point of the aluminum alloy ingot to be treated through differential scanning calorimetry analysis; then putting the mixture into a heat treatment furnace, raising the temperature from room temperature to a temperature above the eutectic temperature with a low melting point in stages, keeping the temperature below the melting point for 6 hours; when the temperature is lower than 580 ℃, the heating speed is 8 ℃/min, and after the temperature is raised to 580 ℃, the heating speed is 4 ℃/min; heating to 610 ℃, and then preserving heat for 6 h;
and step 3: and (3) rapid cooling: and taking out the sample, and putting the sample into ice water for quenching.
Example 2
A high-temperature treatment method of an aluminum alloy with a low-melting-point eutectic structure comprises the following steps:
step 1: alloy smelting: the aluminum alloy cast ingot comprises the following components in percentage by weight: the zinc content was 4% in addition to aluminum; the indium content is 0.01%; the erbium content was 4%.
(1) Putting a proper amount of pure aluminum into the crucible for cleaning and preheating the crucible, heating the crucible to 750 ℃, pouring the whole crucible by using an iron ladle coated with a protective coating after the pure aluminum is fully melted, standing for 30min, and pouring out; (2) putting all aluminum ingots into the crucible, and then heating; after the temperature is raised to 750 ℃, putting Al-Er intermediate alloy after the aluminum ingot is completely melted; (3) keeping the temperature unchanged, and adding the Al-Zn intermediate alloy after the Al-Er intermediate alloy is completely melted; (4) keeping the temperature unchanged, adding C accounting for 1 percent of the total weight of the alloy in the crucible after the Al-Zn intermediate alloy is completely melted2Cl6Refining, stirring thoroughly, and standing for 15min, skimming slag by using an iron ladle coated with a protective coating; keeping the temperature unchanged, and adding Al-In intermediate alloy; casting the melt at 740 ℃ to obtain an aluminum alloy ingot;
step 2: high-temperature treatment: firstly, determining the low-melting-point eutectic temperature and the melting point of the aluminum alloy ingot to be treated through differential scanning calorimetry analysis; then putting the mixture into a heat treatment furnace, raising the temperature from room temperature to a temperature above the eutectic temperature with a low melting point in stages, keeping the temperature below the melting point for 8 hours; when the temperature is lower than 580 ℃, the heating speed is 5 ℃/min, and after the temperature is raised to 580 ℃, the heating speed is 2 ℃/min; heating to 620 ℃, and then carrying out heat preservation for 8 h;
and step 3: and (3) rapid cooling: and taking out the sample, and putting the sample into ice water for quenching.
Example 3
A high-temperature treatment method of an aluminum alloy with a low-melting-point eutectic structure comprises the following steps:
step 1: alloy smelting: the aluminum alloy cast ingot comprises the following components in percentage by weight: the zinc content was 3% in addition to aluminum; the indium content is 0.02%; the erbium content was 0.6%.
(1) Putting a proper amount of pure aluminum into the crucible for cleaning and preheating the crucible, heating the crucible to 750 ℃, pouring the whole crucible by using an iron ladle coated with a protective coating after the pure aluminum is fully melted, standing for 15min, and pouring out; (2) putting all aluminum ingots into the crucible, and then heating; after the temperature is raised to 800 ℃, putting Al-Er intermediate alloy after the aluminum ingot is completely melted; (3) keeping the temperature unchanged, and adding the Al-Zn intermediate alloy after the Al-Er intermediate alloy is completely melted; (4) keeping the temperature unchanged, adding C accounting for 2 percent of the total weight of the alloy in the crucible after the Al-Zn intermediate alloy is completely melted2Cl6Refining, stirring thoroughly, standing for 10min, and removing slag with an iron ladle coated with a protective coating; keeping the temperature unchanged, and adding Al-In intermediate alloy; casting the melt at 760 ℃ to obtain an aluminum alloy ingot;
step 2: high-temperature treatment: firstly, determining the low-melting-point eutectic temperature and the melting point of the aluminum alloy ingot to be treated through differential scanning calorimetry analysis; then putting the mixture into a heat treatment furnace, raising the temperature from room temperature to a temperature above the eutectic temperature with a low melting point in stages, keeping the temperature below the melting point for 8 hours; when the temperature is lower than 580 ℃, the heating speed is 10 ℃/min, and after the temperature is raised to 580 ℃, the heating speed is 5 ℃/min; heating to 630 ℃, and then carrying out heat preservation for 4 h;
and step 3: and (3) rapid cooling: and taking out the sample, and putting the sample into liquid nitrogen for quenching.
The test method comprises the following steps:
the heat-treated sample of example 2 was processed into a diameter of 14 mm. times.8 mm. Observing the alloy structure by using a Hitachi SU8020 scanning electron microscope; the polarization curve was tested by a Gamry750 electrochemical workstation.
Results and analysis:
(1) sample tissue analysis
FIG. 2 is an SEM picture of an as-cast Al-Zn-In-1Er alloy and a quenched alloy after heat preservation at 620 ℃ for 8h, wherein grain boundary segregation of a sample before heat treatment is serious, most of precipitates are distributed on the grain boundary In a chain shape and an intermittent net shape, and a small part of precipitates are distributed on a solid solution In a granular shape. In the alloy structure after high-temperature treatment, continuous chain precipitates basically disappear, and instead, spherical and punctate precipitates are dispersedly distributed on an alpha-Al matrix. The dissolution phenomenon of the chain phase of the grain boundary after the high temperature treatment was explained, and at the same time, a spherical phase was precipitated in the matrix.
(2) Polarization curve analysis
FIG. 3 is an electrochemical polarization curve of the alloy, and Table 1 is Tafel curve fitting values of the alloy. As can be seen, the as-cast sample had the lowest self-corrosion potential, and the water-cooled samples had self-corrosion potentials of-1016 mV, respectively. Compared with the as-cast alloy, the corrosion potential of the alloy after heat treatment has obvious negative shift. It can be seen from fig. 3 that, in the Tafel polarization overpotential range, the slopes of the anodic polarization curves of the alloys in the two states are both small, i.e., the degree of anodic polarization is small, which indicates that the alloys can achieve continuous active dissolution before and after heat treatment without an obvious passivation interval. The sample after heat treatment has less polarization than the as-cast sample, low self-corrosion potential and effective cathodic protection.
The polarization curves of the aluminum alloy materials prepared in example 2 before and after heat treatment are fitted, and the specific data are shown in table 1.
The results of the polarization curve fit in Table 1 show the self-corrosion current density I of the heat treated alloy compared to the as-cast alloycorrElevated, self-etching current density Icorr46.31. mu.A was reached. The increase of the self-corrosion current density shows that the alloy has high reaction activity and is beneficial to cathodic protection. As can be seen from the data in Table 1, the alloy material prepared in example 2 has more uniform structure, reduced self-corrosion potential, increased self-corrosion current density and better anode performance after high-temperature treatment.
TABLE 1
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (4)
1. A high-temperature treatment method of an aluminum alloy with a low-melting-point eutectic structure is characterized by comprising the following steps: the method comprises the following steps: (1) firstly, determining the low-melting-point eutectic temperature and the melting point of the aluminum alloy cast ingot to be treated through differential scanning calorimetry analysis; (2) putting the aluminum alloy cast ingot into a heat treatment furnace, heating the aluminum alloy cast ingot from room temperature to a temperature above the eutectic temperature with a low melting point and below the melting point, then preserving the heat for 4-8 hours, taking out and quenching; the aluminum alloy cast ingot comprises the following components in percentage by mass: zn is less than or equal to 5, In is less than or equal to 0.03, Er0.6-4 and the balance of Al;
heating to 0-20 deg.C above low-melting point eutectic temperature, and keeping the temperature below the melting point temperature;
when the temperature of the aluminum alloy cast ingot is lower than 580 ℃, the heating rate is 5-10 ℃/min; when the temperature of the aluminum alloy cast ingot is higher than 580 ℃, the heating rate is 2-5 ℃/min;
the high-temperature treatment method comprises the following specific steps:
(1) putting an aluminum ingot into the crucible, and then heating; when the temperature is raised to 750-;
(2) keeping the temperature unchanged, and adding the Al-Zn intermediate alloy after the Al-Er intermediate alloy is completely melted;
(3) keeping the temperature unchanged, adding a refining agent after the Al-Zn intermediate alloy is completely melted, fully stirring, and then standing for 10-15 min;
(4) keeping the temperature unchanged, adding the Al-In intermediate alloy, and casting after the Al-In intermediate alloy is completely melted.
2. The high-temperature treatment method of an aluminum alloy having a low-melting-point eutectic structure according to claim 1, wherein: before the aluminum ingot is put into the crucible, a proper amount of pure aluminum is put into the crucible, the temperature is raised to 750 ℃, the whole crucible is poured by a spoon after the pure aluminum is fully melted, and then the whole crucible is kept stand for 15-30min and poured out.
3. The high-temperature treatment method of an aluminum alloy having a low-melting-point eutectic structure according to claim 1, wherein: the casting was carried out at a temperature of 740 and 760 ℃.
4. The high-temperature treatment method of an aluminum alloy having a low-melting-point eutectic structure according to claim 1, wherein: the refining agent is C2Cl6, and the addition amount of the refining agent is 0.5-2% of the total weight of the alloy in the crucible.
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