WO2015109893A1 - Alliage de séries al-mg-si-cu-zn de type à réaction de viellissement rapide et son procédé de préparation - Google Patents

Alliage de séries al-mg-si-cu-zn de type à réaction de viellissement rapide et son procédé de préparation Download PDF

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WO2015109893A1
WO2015109893A1 PCT/CN2014/092698 CN2014092698W WO2015109893A1 WO 2015109893 A1 WO2015109893 A1 WO 2015109893A1 CN 2014092698 W CN2014092698 W CN 2014092698W WO 2015109893 A1 WO2015109893 A1 WO 2015109893A1
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alloy
aging
treatment
novel
response characteristics
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PCT/CN2014/092698
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Chinese (zh)
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郭明星
庄林忠
张济山
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北京科技大学
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/10—Alloys based on aluminium with zinc as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/18—Alloys based on aluminium with copper as the next major constituent with zinc
    • 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
    • C22F1/04—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

Definitions

  • the invention belongs to the technical field of aluminum alloys, relates to a novel Al-Mg-Si-Cu-Zn alloy which can be industrially applied and a preparation method thereof, and is specially developed for an aluminum alloy with rapid aging response characteristics which is urgently needed in the automobile field, and can be developed. To ensure the high requirements of high forming performance and high baking hardening performance of aluminum alloy for automobile lightweight body.
  • Typical aluminum alloys for automobile body panels are 2xxx, 5xxx and 6xxx alloys, of which 6xxx alloys are commonly used in AA6009, AA6010, AA6016, AA6111 and AA6022.
  • the heat-treating Al-Mg-Si alloy has good comprehensive performance, it has been found in the research and application process that the alloy has good forming property if it is directly subjected to solution hardening treatment at 500-570 °C. However, most of the actual production process needs to transport the sheet to the automobile manufacturer for subsequent stamping. During this period, the alloy sheet will have a certain degree of strength rise during the natural placement process, which will reduce the forming properties of the alloy sheet and the subsequent Baking hardening performance, this phenomenon is called the natural aging deterioration effect.
  • the preparation process commonly used in the preparation process of 6xxx series aluminum alloys for automobiles is as follows: alloy smelting casting ⁇ homogenization ⁇ hot rolling ⁇ cold rolling ⁇ solid solution ⁇ pre-aging (T4P treatment) ⁇ stamping ⁇ brushing ⁇ 170- 185 ° C paint processing and other processes. Due to the special nature of automobile sheet preparation, it is inevitable that the alloy has a lower strength in the T4P state before forming, and the alloy strength can be greatly improved during the baking process (ie, T8X state), thus ensuring the alloy sheet has a higher quality. Good resistance to dents, etc., so alloy composition design and heat treatment process development is the key way to solve this problem.
  • MgZn 2 strengthening phase can greatly increase the strength of the Al-Zn-Mg-Cu alloy, it is possible to simultaneously utilize two main strengthening phases of the Al-Mg-Si and Al-Zn-Mg-Cu alloys.
  • Mg 2 Si and MgZn 2 or their transition phase act as a strengthening phase of the novel Al-Mg-Si alloy, achieving multiphase synergistic precipitation and achieving multiphase synergistic strengthening.
  • the developed alloy will definitely exhibit excellent fast aging. Response characteristics.
  • the present invention is based on this design idea to carry out new alloy composition design and process development.
  • the present invention develops a novel Al-Mg-Si-Cu-Zn with rapid aging response characteristics in view of the fact that the conventional Al-Mg-Si alloy has insufficient aging response speed and age hardening property.
  • the alloy is fully utilized by the multiphase synergistic precipitation and synergistic strengthening of Mg 2 Si and MgZn 2 to greatly improve the overall performance of the alloy.
  • the alloy of the invention is particularly suitable for the manufacture of an aluminum alloy for an automobile body outer panel, and has excellent paint hardening performance after the outer panel of the vehicle body is formed by press molding.
  • the invention first selects the composition range of the Al-Mg-Si-Cu-Zn alloy with multi-phase structure by component design and optimization, and then prepares the designed alloy through the process of smelting casting and studies the aging precipitation behavior.
  • the new Al-Mg-Si-Cu-Zn alloy composition with fast aging response was finally determined.
  • the specific preparation process is as follows: FactSage phase diagram calculation ⁇ Al-Mg-Si alloy composition selection ⁇ alloy preparation and smelting casting ⁇ ingot homogenization ⁇ hot rolling deformation ⁇ intermediate annealing ⁇ cold rolling deformation ⁇ solution quenching ⁇ multi-stage aging deal with.
  • a first object of the present invention is to provide a novel Al-Mg-Si-Cu-Zn series aluminum alloy having fast aging response characteristics, characterized in that the chemical composition and mass percentage of the alloy are: Zn: 0.10. ⁇ 3.7 wt%, Mg 0.3 to 1.2 wt%, Si 0.3 to 1.2 wt%, Cu 0.05 to 0.7 wt%, Fe ⁇ 0.3 wt%, Mn ⁇ 0.3 wt%, Cr ⁇ 0.2 wt%, Ti ⁇ 0.2 wt%, The balance is Al.
  • the chemical composition has a Zn content ranging from 0.4 to 3.5% by weight.
  • the mass ratio of Mg/Si of the chemical components Mg and Si ranges from 0.5 to 1.
  • the chemical composition of Si and Cu ranges from 0.8 to 1.1 wt% of Si and 0.15 to 0.35 wt% of Cu.
  • a second object of the present invention is to provide a method for preparing the above-mentioned novel Al-Mg-Si-Cu-Zn series aluminum alloy having rapid aging response characteristics, the preparation method comprising the following steps:
  • Step one smelting casting
  • Step three hot rolling deformation
  • Step four intermediate annealing
  • Step five cold rolling deformation
  • Step 6 Solution treatment above 540 ° C;
  • Step seven water quenching treatment
  • Step eight multi-level aging treatment.
  • the two-stage homogenization of the second step is specifically: the alloy sample after the smelting and casting is started to be heated from room temperature to 470-485 ° C for 2 to 5 hours at a temperature increase rate of 20 to 40 ° C / h, and then 20 ⁇ 40 °C / h continue to raise the temperature to 545 ⁇ 555 ° C for 14 ⁇ 20h, and finally at 20 ⁇ 40 ° C / h cooling rate with the furnace when the temperature is reduced to 100 ° C.
  • the hot rolling deformation of the third step is specifically: the rolling temperature is 545-555 ° C, the total hot rolling deformation is >90%, and the finishing rolling temperature is ⁇ 300 ° C;
  • the intermediate annealing in the fourth step is specifically: the alloy sample after hot rolling deformation is directly placed in a heat treatment furnace at 350 to 450 ° C for intermediate annealing for 1 to 3 hours, and then air cooled.
  • the total cold rolling deformation of the cold rolling deformation in the step 5 is between 50% and 75%, and the pass reduction is between 15% and 25%.
  • the solution treatment of 540 ° C or more in the step 6 is specifically: performing a solution treatment in a salt bath furnace at 545 to 555 ° C / 1-6 min; and the water quenching treatment in the step 7 is a solution treatment; The subsequent alloy sample was directly subjected to water quenching.
  • the multi-stage aging treatment of the step 8 is: transferring the water-quenched alloy sample to the pre-aging furnace for pre-aging treatment at 70-140 ° C / 9-15 h in 2 to 5 min, and then Leave at room temperature for 14 days, and finally perform artificial aging at 185 °C; or transfer the alloy sample after water quenching to a 70-140 °C pre-aging furnace at a cooling rate of 1-15 °C / h to 2 to 5 minutes. It was taken out at 20 to 40 ° C, then left at room temperature for 14 days, and finally subjected to artificial aging at 185 ° C.
  • the present invention has the following advantages: the novel Al-Mg-Si-Cu-Zn alloy of the present invention can fully utilize the elements of the main alloying elements Mg, Si, Cu and Zn in the matrix. Interaction, through a suitable heat treatment regulation, a variety of strengthening phases are synergistically precipitated. Finally, a large number of different types of strengthening phases are uniformly dispersed in the alloy matrix, so that the alloy can obtain a large intensity increase in a short aging time, that is, Achieve the so-called fast aging response characteristics.
  • the alloy of the invention is very suitable for further development and production of aluminum alloy outer panel materials for automobiles which are currently studied.
  • Fig.1 shows the hardness change law of artificial aging immediately after solid solution quenching of several new aluminum alloys.
  • Fig. 2 shows the law of hardness change of natural aging after several kinds of new aluminum alloys are solution-quenched.
  • Figure 3 shows the results of DSC analysis after 14 days of natural aging after solid solution quenching of several new aluminum alloys.
  • Fig. 4 shows the change of hardness of several new aluminum alloys after solid solution quenching after natural aging for 14 days and then artificial aging at 185 °C.
  • Figure 5 shows the variation of hardness of several new aluminum alloys during natural aging after pre-aging treatment.
  • Figure 6 shows the results of DSC analysis of several new aluminum alloys after 14 days of pre-aging + natural aging.
  • Fig. 7 shows the change of hardness of several new aluminum alloys after pre-aging + natural aging for 14 days and then at 185 °C.
  • Fig. 8 TEM microstructure of the T4P alloy 5# alloy heated to 250 ° C at 10 ° C / min.
  • the raw materials were respectively 99.9 wt% of high purity aluminum, industrial pure Mg, industrial pure Zn, intermediate alloy Al-20 wt% Si, Al-50 wt% Cu, Al-20 wt% Fe, Al-10 wt% Mn, and the like.
  • the specific smelting process in the resistance furnace is to first add pure aluminum to the crucible, set the furnace temperature to 850 ° C, and add Al-20 wt% Si, Al-50 wt% Cu, Al-20 wt% Fe after the pure aluminum is melted.
  • the measured value of the component is higher than the design value, a certain amount of metal pure aluminum is appropriately added according to the excess value for dilution; After rising to 740 ° C, slag is added, and a refining agent is added for degassing refining; then, when the melt temperature is lowered to about 720 ° C, Al-5 wt% Ti-1 wt% B grain refiner is added and stirred appropriately, and finally After the temperature is kept for 10 minutes, the melt is cast to four. Within a water-cooled steel.
  • Table 1 The specific chemical compositions of the inventive alloys are shown in Table 1.
  • Table 1 shows the chemical composition of the alloy of the invention (mass percentage, wt%)
  • the invention ingot is homogenized in a circulating air furnace, and the treatment process is: placing the alloy ingot into a circulating air furnace, turning on the power supply, and starting to heat up at a heating rate of 20 to 70 ° C / h, until the temperature reaches 460 to 490 °C for 1 ⁇ 7h, and then continue to raise the temperature to 540 ⁇ 560 ° C for 10 ⁇ 25h at 20 ⁇ 70 ° C / h, and then take the temperature drop of 20 ⁇ 70 ° C / h with the furnace to 100 ° C when the sample is taken out; Then the ingot is subjected to hot rolling deformation ⁇ intermediate annealing ⁇ cold rolling deformation for better optimization.
  • the homogenization treatment is carried out, and the treatment process is as follows: the temperature rise starts at a temperature increase rate of 20 to 40 ° C / h, and the temperature is maintained at 470 to 485 ° C for 2 ⁇ 5h, then continue to raise the temperature to 545 ⁇ 555 ° C for 14 ⁇ 20h at 20 ⁇ 40 ° C / h, and then take the sample at the temperature drop rate of 20 ⁇ 40 ° C / h when the furnace is cooled to 100 ° C.
  • the sample is directly cut out on the homogenized block material and placed in a salt bath furnace for solution treatment at 545-555 ° C / 1-6 min (ie, 1-6 min in a salt bath furnace at 545-555 ° C).
  • the solution treatment and water quenching treatment were carried out directly into the 185 ° C aging furnace for artificial aging at different times to compare the aging precipitation behavior of various alloys (see Figure 1 for details).
  • the homogenization treatment is carried out, and the treatment process is as follows: the temperature rise starts at a temperature increase rate of 20 to 40 ° C / h, and the temperature reaches 470. Heat at ⁇ 485°C for 2 ⁇ 5h, then continue to raise the temperature to 545 ⁇ 555°C for 14 ⁇ 20h at 20 ⁇ 40°C/h, then take off the sample when the temperature is lowered to 100°C with the cooling rate of 20 ⁇ 40°C/h. .
  • the sample is directly cut out on the homogenized block material and placed in a salt bath furnace for 545-555 ° C / 1-6 min solution and water quenching treatment, and then directly subjected to natural aging at room temperature to measure the alloy.
  • the change of hardness with natural aging time see Figure 2 for details.
  • the DSC analysis was carried out on the 14-day natural aging sample.
  • the specific implementation scheme was as follows: a disc having a diameter of 3 mm ⁇ 1 mm and a mass of about 15 mg was cut out, and differential scanning analysis was performed by differential scanning calorimeter Q2000 (DSC). High purity Al was used as a standard and heated from 20 ° C to 400 ° C at a heating rate of 10 ° C / min. Based on this, the difference in aging precipitation behavior of different alloys is further grasped (see Figure 3 for details).
  • the homogenization treatment is carried out, and the treatment process is as follows: the temperature rise starts at a temperature increase rate of 20 to 40 ° C / h, and the temperature reaches 470. Heat at ⁇ 485°C for 2 ⁇ 5h, then continue to raise the temperature to 545 ⁇ 555°C for 14 ⁇ 20h at 20 ⁇ 40°C/h, then take off the sample when the temperature is lowered to 100°C with the cooling rate of 20 ⁇ 40°C/h. .
  • the sample is directly cut out on the homogenized block material and placed in a salt bath furnace for 545-555 ° C / 1-6 min solution and water quenching treatment, and then subjected to natural aging for 14 days at room temperature (T4 State), the natural aging samples were subjected to artificial aging treatment at 185 ° C for different times to measure the hardness change of the alloy (see Figure 4 for details).
  • the homogenization treatment is carried out, and the treatment process is as follows: the temperature rise starts at a temperature increase rate of 20 to 40 ° C / h, and the temperature reaches 470. Heat at ⁇ 485°C for 2 ⁇ 5h, then continue to raise the temperature to 545 ⁇ 555°C for 14 ⁇ 20h at 20 ⁇ 40°C/h, then take off the sample when the temperature is lowered to 100°C with the cooling rate of 20 ⁇ 40°C/h. .
  • the sample is directly cut out on the homogenized block material and placed in a salt bath furnace for 545-555 ° C / 1-6 min solution and water quenching treatment, and then transferred to the pre-aging furnace within 2 to 5 minutes.
  • the pre-aging treatment is carried out at 70-140 ° C / 9 ⁇ 15 h, and finally the pre-aging sample is subjected to natural aging at room temperature, and the variation of the hardness of the alloy with the natural aging time is measured (as shown in Fig. 5).
  • a corresponding DSC analysis was also carried out.
  • the specific implementation scheme is: cutting a wafer with a diameter of 3 mm ⁇ 1 mm and a mass of about 15 mg, using a differential scanning calorimeter Q2000 (DSC) Differential thermal analysis was performed using high purity Al as a standard and heating from 20 ° C to 400 ° C at a heating rate of 10 ° C / min. The corresponding DSC curve is shown in Figure 6.
  • DSC differential scanning calorimeter Q2000
  • the homogenization treatment is carried out, and the treatment process is as follows: the temperature rise starts at a temperature increase rate of 20 to 40 ° C / h, and the temperature reaches 470. Heat at ⁇ 485°C for 2 ⁇ 5h, then continue to raise the temperature to 545 ⁇ 555°C for 14 ⁇ 20h at 20 ⁇ 40°C/h, then take off the sample when the temperature is lowered to 100°C with the cooling rate of 20 ⁇ 40°C/h. .
  • the sample is directly cut out on the homogenized block material and placed in a salt bath furnace for 545-555 ° C / 1-6 min solution and water quenching treatment, and then transferred to the pre-aging furnace within 2 to 5 minutes.
  • the pre-aging treatment is carried out at 70-140 ° C / 9-15 h, and the pre-aging sample is placed at room temperature for 14-angstrom alloy to be stable (ie, T4P (1) state), and finally the T4P (1) state sample is subjected to 185 ° C artificial aging treatment at different times, measuring the hardness change of the alloy (see Figure 7 for details).
  • the homogenization treatment is carried out, and the treatment process is as follows: the temperature rise starts at a temperature increase rate of 20 to 40 ° C / h, and the temperature reaches 470. Heat at ⁇ 485°C for 2 ⁇ 5h, then continue to raise the temperature to 545 ⁇ 555°C for 14 ⁇ 20h at 20 ⁇ 40°C/h, then take off the sample when the temperature is lowered to 100°C with the cooling rate of 20 ⁇ 40°C/h. .
  • the sample is directly cut out on the homogenized block material and placed in a salt bath furnace for 545-555 ° C / 1-6 min solution and water quenching treatment, and then transferred to 70-140 within 2 to 5 minutes.
  • the temperature is lowered to 20 ⁇ 40 °C at a cooling rate of 1-15 °C/h, and the pre-aging sample is placed at room temperature for 14-amber alloy performance (ie T4P(2) state), and finally The T4P (2) sample was subjected to artificial aging treatment at 185 ° C / 20 min, and the hardness increment of the alloy was measured (see Table 2 for details).
  • the homogenization treatment is carried out, and the treatment process is as follows: the temperature is raised at a heating rate of 20 to 40 ° C / h, and the temperature is maintained at 470 to 485 ° C for 2 to 5 hours, and then Continue to heat up at 20 ⁇ 40 ° C / h The sample was incubated at 545-555 ° C for 14-20 h, and then the sample was taken out at a cooling rate of 20-40 ° C/h as the furnace was cooled to 100 ° C. After homogenization, the ingot is cut into a face and reheated to 545-555 °C for hot rolling.
  • the total deformation of hot rolling is >90%, the final rolling temperature is ⁇ 300 °C, and the thickness of hot rolling finishing is 4.0 mm;
  • the back sheet is annealed at 350-450 ° C / 1-3 h, then cold rolled to 1 mm thick, the pass reduction is 15-25%, and the total deformation is 75%;
  • the cold rolled sheet is 545 ⁇ 555 ° C / 1-6 min solution and water quenching treatment, and then ensure that within 2 ⁇ 5min transfer to 70-140 ° C pre-aging furnace at a cooling rate of 1-15 ° C / h to cool down to 20 ⁇ 40 ° C to take out,
  • the pre-aging samples were placed at room temperature for 14-star alloy stability (ie T4P(2) state), and finally T4P(2) samples were subjected to artificial aging treatment at 185 °C/20 min to measure T4P(2).
  • Tensile properties of alloys and high temperature artificial aging alloys see Table 3 for details).
  • the Al-Mg-Si-Cu alloy after the addition of element Zn has a high temperature aging precipitation rate. Accelerated, but with the change of Zn content, the aging precipitation rate is quite different, which is mainly due to the influence of the content of each main alloy element on its interaction. Although the addition of a certain amount of element Zn can accelerate the high temperature aging precipitation rate of the T4 alloy, the precipitation rate is still not ideal. If the alloy is subjected to the corresponding pre-aging treatment (Example 4), the performance of several alloys is relatively stable during room temperature placement, and similar to the Zn-free 1# alloy, the solid solution quenched alloy does not appear in natural aging. The hardness rise in the process (as shown in Fig.
  • the present invention optimizes the interaction between the main alloying elements Mg, Si, Cu and Zn in the novel Al-Mg-Si-Cu-Zn alloy by optimizing the composition design and processing heat treatment process.
  • the ground control makes the alloy have more excellent fast aging response characteristics than the conventional Al-Mg-Si alloy.
  • the newly developed preparation process not only accelerates the aging response of the alloy, but also suppresses the natural aging deterioration effect of the solution-quenched Al-Mg-Si alloy, so that the alloy sheet has excellent formability and paint hardening property.
  • the alloy and the process of the invention are not only very suitable for the manufacture of aluminum alloy for automobile lightweight body panels, but also have certain guiding significance for the development, processing and application of new aluminum alloys with fast aging response in other fields, and it is worthwhile.
  • Automobile manufacturers and aluminum alloy companies pay attention to the alloys and related preparation processes of the invention, so that they can be promoted and applied in this field as soon as possible.

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Abstract

L'invention concerne un alliage de séries AL-MG-SI-CU-ZN à réaction de viellissement rapide et son procédé de préparation Les composants chimiques de l'alliage et leur teneur en pourcentage en masse sont : Zn : 0,10-3,7 % , Mg : 0,3-1,2 %, Si : 0,3-1,2 %, Cu: 0,05-0,7 %, Fe ≤ O,3 %, Mn ≤ 0,3 %, Cr ≤ 0,2 %, Ti ≤ 0,2 %, le reste étant Al. L'alliage est produit par mise en solution après laminage à chaud et laminage à froid, puis par exécution d'une trempe à l'eau et d'un traitement de vieillissement multi-étage.
PCT/CN2014/092698 2014-01-22 2014-12-01 Alliage de séries al-mg-si-cu-zn de type à réaction de viellissement rapide et son procédé de préparation WO2015109893A1 (fr)

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CN201410030681.6 2014-01-22

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