WO2023125282A1 - High-plasticity composite modified aluminum alloy part and preparation method therefor - Google Patents

High-plasticity composite modified aluminum alloy part and preparation method therefor Download PDF

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Publication number
WO2023125282A1
WO2023125282A1 PCT/CN2022/141397 CN2022141397W WO2023125282A1 WO 2023125282 A1 WO2023125282 A1 WO 2023125282A1 CN 2022141397 W CN2022141397 W CN 2022141397W WO 2023125282 A1 WO2023125282 A1 WO 2023125282A1
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aluminum
alloy
aluminum alloy
titanium
rare earth
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PCT/CN2022/141397
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French (fr)
Chinese (zh)
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彭珞洲
答建成
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上海耀鸿科技股份有限公司
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Priority to EP22914536.2A priority Critical patent/EP4321641A1/en
Priority to KR1020237039152A priority patent/KR20230170749A/en
Publication of WO2023125282A1 publication Critical patent/WO2023125282A1/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
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/026—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • 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
    • 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
    • C22F1/043—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 of alloys with silicon as the next major constituent

Definitions

  • the invention relates to the technical field of alloy materials and preparation, in particular to a high-plastic composite modified aluminum alloy product and a preparation method thereof.
  • Aluminum alloy is the most widely used non-ferrous metal structural material in industry, and has been widely used in aviation, aerospace, automobile, machinery manufacturing, shipbuilding and chemical industry.
  • Cast aluminum alloy has the characteristics of casting fluidity, good air tightness, small shrinkage rate and small thermal cracking tendency, etc., and it has become the first choice material for lightweight automobile wheels.
  • aluminum alloy wheel parts require medium strength and higher ductility to avoid instantaneous fracture of the wheel in the event of frontal impact and side impact (within the design load bearing range).
  • the present invention provides a high-plastic composite modified aluminum alloy product and a preparation method thereof, which can further improve the plasticity and mechanical strength of the aluminum alloy.
  • Step S1 providing an aluminum alloy melt
  • Step S2 providing a modifier
  • the modifier is a combination of rare earth aluminum alloy, aluminum-strontium master alloy, aluminum-titanium or aluminum-titanium-boron master alloy,
  • the modifier is a combination of composite rare earth aluminum alloy, aluminum titanium or aluminum titanium boron intermediate alloy, and the composite rare earth aluminum alloy contains strontium, titanium or titanium boron, and rare earth metals,
  • the rare earth metal in the rare earth aluminum alloy and the composite rare earth aluminum alloy is any one or more of lanthanum, cerium, and yttrium;
  • Step S3 adding the modifying agent to the aluminum alloy melt under an inert gas atmosphere and melting to obtain a modified aluminum alloy melt;
  • Step S4 using the modified aluminum alloy melt to perform casting to obtain the cast aluminum alloy biscuit;
  • Step S5 performing heat treatment on the aluminum alloy green body, wherein the heat treatment includes:
  • Water quenching treatment adding the aluminum alloy biscuit after solid solution treatment into a water bath at a temperature of 60-70°C, and quenching water for 2-4 minutes;
  • step S1 includes:
  • composition of the aluminum alloy master ingot is hypoeutectic aluminum alloy or eutectic aluminum alloy.
  • the modifier is a combination of rare earth aluminum alloy, aluminum-strontium master alloy, aluminum-titanium or aluminum-titanium-boron master alloy, wherein the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium The boron master alloy is added at intervals,
  • the rare earth aluminum alloy is added first, or added together with the first added party, or added between the addition of the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy.
  • step S3 includes:
  • Step S301 adding the rare earth aluminum alloy into the aluminum alloy melt and melting to obtain a first homogeneously mixed melt
  • Step S302 adding the aluminum-strontium master alloy into the first homogeneously mixed melt and continuing to smelt to obtain a second homogeneously mixed melt;
  • Step S303 adding the aluminum-titanium or aluminum-titanium-boron master alloy into the second homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
  • the modifying agent is a combination of composite rare earth aluminum alloy, aluminum titanium or aluminum titanium boron master alloy, and the step S3 includes:
  • Step S310 adding the composite rare earth aluminum alloy into the aluminum alloy melt and melting to obtain a fourth uniformly mixed melt
  • Step S320 adding the aluminum-titanium or aluminum-titanium-boron master alloy into the fourth homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
  • the preparation of the composite rare earth aluminum alloy includes:
  • Step S211 providing the aluminum melt
  • Step S212 providing an aluminum-strontium master alloy, an aluminum-titanium or aluminum-titanium-boron master alloy, and a rare earth aluminum master alloy, wherein the rare earth metal in the rare earth aluminum master alloy is one or more selected from lanthanum, cerium, and yttrium;
  • Step S213 under an inert gas atmosphere, sequentially add the rare earth aluminum master alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy into the aluminum melt and melt to obtain the composite rare earth alloy.
  • the modifier accounts for 0.4-0.6wt% of the total amount of the modified aluminum alloy melt, and the mass ratio of the rare earth metal: strontium: titanium or the total amount of titanium boron is 1: (0.1-1.2) : (0.1-1.2).
  • the heating rate in the solution treatment is controlled at 1.5-3° C./min, and the holding time is controlled at 120-180 min.
  • the solid solution treatment, the quenching treatment, and the aging treatment are continuous treatments, and the water bath is a circulating water bath. After the quenching treatment, before the aging treatment, the cast aluminum The temperature of the alloy green body is kept above 55°C.
  • the temperature is raised from 110-140°C to 160-200°C at a heating rate of 2-4°C/min, and then naturally cooled to room temperature.
  • the high-plastic composite modified aluminum alloy product according to the second aspect of the present invention is prepared by the preparation method described in any of the above-mentioned embodiments, and the tensile strength of the high-plastic composite modified aluminum alloy product is: 280MPa or more, the yield strength is 200MPa or more, and the elongation is 12% or more.
  • the aluminum alloy is modified by introducing rare earth metals, and the casting is treated in combination with a specific heat treatment process, so that its plasticity (elongation rate) can be greatly improved ), reduce the occurrence of brittle cracks, and at the same time improve its mechanical strength to meet the needs of aviation, aerospace, and automotive fields.
  • Fig. 1 is the metallographic structure image of aluminum alloy parts in different stages, wherein, (a) is the image of A356 aluminum alloy before heat treatment, (b) is the image of A356 aluminum alloy after heat treatment, (c) is embodiment 1 In (d) is the image after compound modification and heat treatment in Example 1.
  • Step S1 providing an aluminum alloy melt.
  • an aluminum alloy melt is prepared.
  • Purification treatment may include the following steps, for example:
  • Step S11 providing an aluminum alloy ingot
  • Step S12 removing the oxide layer on the surface of the aluminum alloy ingot
  • Step S13 cleaning and drying the aluminum alloy ingot from which the scale layer has been removed
  • Step S14 melting the dried aluminum alloy ingot to obtain an initial melt
  • Step S15 refining the initial melt to obtain the aluminum alloy melt.
  • the oxide scale layer on the surface is first removed, then cleaned to remove surface scum, smelted after drying, and the melt is refined.
  • the specific refining process will be described in detail later.
  • undesired impurities such as Fe, oxides, etc. can be removed. It is beneficial to further improve the modification and refinement of rare earth alloys.
  • Fe and its oxides can be removed by adding manganese or aluminum-manganese alloy to form surface scum, for example.
  • the aluminum alloy melt for example, it may be an aluminum-magnesium alloy, an aluminum-silicon alloy, an aluminum-silicon-magnesium alloy, etc., which is not specifically limited in the present invention.
  • Step S2 providing a modifier.
  • the modifier is a combination of rare earth aluminum alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy, or the modifier is a combination of compound rare earth aluminum alloy, aluminum titanium or aluminum titanium boron master alloy ,
  • the composite rare earth aluminum alloy contains strontium, titanium or titanium boron, and rare earth metals,
  • the rare earth metal in the rare earth aluminum alloy and the composite rare earth aluminum alloy is any one or more of lanthanum, cerium, and yttrium.
  • the modifier is a combination of rare earth aluminum alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy.
  • the aluminum-strontium master alloy is the modifier
  • the aluminum-titanium master alloy or the aluminum-titanium-boron master alloy is the refiner. That is, conventional modifiers and refiners can be used.
  • the modifier and/or the refiner commercially available materials can be used, or the corresponding metal strontium, titanium, titanium & boron can be weighed and melted in aluminum melt to form A homogeneous alloy is prepared.
  • rare earth aluminum alloys are further introduced to overcome the limitation of mechanical properties due to the "poisoning" reaction between modifiers and refiners.
  • the rare earth metal in the rare earth aluminum alloy considering the strontium in the modifier and the titanium and boron in the refiner, the group IIIB elements whose electronic structure is in between can be selected. In comprehensive consideration of its stability, resources, etc., preferably, one or more of yttrium, lanthanum in lanthanide metals, and cerium are used.
  • the rare earth aluminum alloy for example, one or more of commercially available Al-10Ce, Al-20Ce, Al-20La, Al-10La, Al-20Y, and Al-10Y can be used.
  • the rare earth aluminum alloy can also be prepared by itself, for example, it can be prepared by the following method:
  • the rare earth aluminum alloy is obtained by standing for a predetermined time and pouring.
  • the aluminum melt can be treated by using commercially available high-purity aluminum ingots with reference to the above-mentioned purification treatment of aluminum alloy ingots, which will not be repeated here.
  • aluminum-strontium master alloys aluminum-titanium master alloys or aluminum-titanium-boron master alloys, and rare-earth aluminum alloys
  • descaling, ultrasonic cleaning, and refining can be performed sequentially, respectively.
  • unwanted impurities and oxides can be further removed, which is beneficial to improving the refinement and modification of the composite rare earth alloy as a product.
  • the modifier is a combination of composite rare earth aluminum alloy, aluminum titanium or aluminum titanium boron master alloy.
  • the composite rare earth aluminum alloy can be prepared by melting and refining the above rare earth aluminum alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy, and aluminum melt.
  • the preparation of the complex rare earth aluminum alloy may include:
  • Step S211 providing aluminum melt
  • Step S212 providing an aluminum-strontium master alloy, an aluminum-titanium or aluminum-titanium-boron master alloy, and a rare earth aluminum alloy, wherein the rare earth metal in the rare earth aluminum alloy is one or more selected from lanthanum, cerium, and yttrium;
  • Step S213 adding the rare earth aluminum alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy into the aluminum melt under an inert gas atmosphere and melting to obtain the composite rare earth alloy.
  • the aluminum-strontium master alloy is added separately from the aluminum-titanium or aluminum-titanium-boron master alloy, and the rare earth aluminum alloy is added before the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy, or It is added together with the first addition, or added between the addition of the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy.
  • the rare earth aluminum alloy, the aluminum-strontium master alloy, the aluminum-titanium or aluminum-titanium-boron master alloy are sequentially added to the aluminum melt at intervals.
  • step S3 under an inert gas atmosphere, the modifier is added to the aluminum alloy melt and smelted to obtain the modified aluminum alloy melt.
  • the modifier is added to the aluminum melt for further melting under an inert gas atmosphere to obtain a modified aluminum alloy melt.
  • the mutual poisoning effect between the modifying agent and the refining agent can be greatly overcome, the addition amount of modifying agent and refining agent can be increased, and at the same time it can Improves the effect of metamorphism and refinement.
  • modifier being a rare earth aluminum alloy, an aluminum strontium master alloy, an aluminum titanium or an aluminum titanium boron master alloy:
  • the rare earth aluminum alloy is added first, or together with the first added party, or at the The aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy are interstitially added.
  • the step S3 may specifically include:
  • Step S301 adding the rare earth aluminum alloy into the aluminum melt and melting to obtain a first homogeneously mixed melt
  • Step S302 adding the aluminum-strontium master alloy into the first homogeneously mixed melt and continuing to smelt to obtain a second homogeneously mixed melt;
  • Step S303 adding the aluminum-titanium or aluminum-titanium-boron master alloy into the second homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
  • the step S3 includes:
  • Step S310 adding the composite rare earth aluminum alloy into the aluminum melt and melting to obtain a fourth homogeneously mixed melt
  • Step S320 adding the aluminum-titanium or aluminum-titanium-boron master alloy into the fourth homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
  • the rare earth aluminum alloy, modifier, refining agent, and aluminum are smelted in advance to obtain a composite rare earth aluminum alloy, it can be prepared by adding it to the above aluminum melt at one time.
  • a refiner to the composite rare earth aluminum alloy when it is completely melted and mixed with the aluminum alloy. That is, aluminum-titanium master alloy or aluminum-titanium-boron master alloy controls grain growth.
  • the modifier preferably accounts for 0.4-0.6 wt% of the total amount of the modified aluminum alloy.
  • the refining in any of the above steps that is, the refining in the process of purifying the aluminum melt, the refining in the process of preparing the rare earth aluminum alloy, and the refining of each melt in the composite rare earth aluminum alloy can be carried out in the following manner:
  • the addition of the refining agent accounts for 0.1 to 0.3% of the mass of the added melt
  • the addition of the slag remover accounts for 0.1 to 0.3% of the mass of the added melt
  • the components of the refining agent contain by mass:
  • the components of the slag remover contain by mass:
  • the hydrogen content is estimated by testing the density of the melt, that is to say, the closer the melt density is to its theoretical density (slightly different according to the different components contained in the alloy, roughly around 2.7g/cm 3 ), then Indicates that the hydrogen contained in it is lower. For example, it can be set that when the density of the melt is less than 2.65g/cm 3 , the refining process is performed; when the density of the melt is greater than or equal to 2.65g/cm 3 , the refining process is not performed or the refining process is terminated. deal with.
  • Step S4 casting the modified aluminum alloy melt to obtain a modified aluminum alloy biscuit.
  • the obtained modified aluminum alloy melt is cast into a mold to obtain the modified aluminum alloy green body.
  • Step S5 performing heat treatment on the modified aluminum alloy biscuit.
  • the inventor has developed a corresponding heat treatment process on the basis of repeated research.
  • the heat treatment includes:
  • Water quenching treatment adding the aluminum alloy biscuit after solid solution treatment into a water bath at a temperature of 60-70°C, and quenching water for 2-4 minutes;
  • the aluminum alloy biscuit is successively subjected to solution treatment, water quenching treatment, and aging treatment.
  • the casting is rapidly cooled, so that the strengthening components are dissolved in the alloy to the maximum extent and then fixed and stored at room temperature.
  • the rise of temperature and the extension of time will result in the recombination of atoms in the supersaturated solid solution lattice, forming a solute atom-enriched region (called the G-PI region) and disappearing of the G-PI region.
  • the atoms of the second phase segregate according to a certain rule and form a G-PII region, forming a metastable second phase (transition phase), a large number of G-PII regions and a small amount of metastable phase combine and the metastable phase transforms into a stable phase ,
  • the second phase particle aggregation The second phase particle aggregation.
  • low-temperature aging is first adopted, so that more phase transitions are in the GP region and the ⁇ 1 region, thereby ensuring sufficient elongation.
  • the heating rate in the solution treatment is controlled at 1.5-3°C/min, and the holding time is controlled at 120-180min.
  • the rose-like ⁇ -Al phase and the rounder spherical ⁇ -Al phase can be further increased, the primary ⁇ -Al phase can be refined, and the number of dendrites can be reduced.
  • the solid solution treatment, the quenching treatment, and the aging treatment are continuous treatments, and the water bath is a circulating water bath.
  • the water bath is a circulating water bath.
  • the temperature is raised from 110-140°C to 160-200°C at a heating rate of 2-4°C/min, and then naturally cooled to room temperature.
  • the cooling rate in the aging treatment stage By controlling the cooling rate in the aging treatment stage, the introduction of defects can be greatly reduced, which helps to improve its plasticity and maintain a high level of mechanical strength.
  • Aluminum alloy aluminum-silicon-magnesium alloy (A356) (purchased from: Shandong Weiqiao Aluminum Industry)
  • High-purity aluminum ingot (purchased from Chinalco, composition: Al (99.99%), Fe ⁇ 0.1%, impurity ⁇ 0.05%)
  • Melting first add the preheated aluminum-silicon-magnesium alloy A356 into the pre-heating melting furnace, and heat and melt it into aluminum water within the range of 760 degrees.
  • Degassing and slag removal After melting into aluminum water, nitrogen (or argon) is introduced and refining agent (0.3wt% refining agent) is blown into the aluminum water, and the ventilation time is controlled at 15 minutes.
  • Al-Sr master alloy purchased from Nantong Angshen Metal Materials Co., Ltd., composition: Al-10Sr, Fe ⁇ 0.05.
  • Pretreatment Use a grinder to clean the scale and surface of the Al-Sr master alloy.
  • Ultrasonic cleaning put the pretreated aluminum-strontium master alloy into an ultrasonic cleaning tank for ultrasonic treatment.
  • Drying put the cleaned aluminum-strontium master alloy into an oven and bake at 60-100°C for 30-60 minutes.
  • Refining treatment After the aluminum-strontium master alloy is melted, it is refined. The molten high-purity aluminum is refined by feeding the Ar+graphite automatic degassing stirring rod. Refining with Ar blowing at 730-750°C for 5-10 minutes, the amount of refining being blown in is 0.1-0.3% of the melt, and kept at 3-5 minutes. During the refining process, there should be no boiling bubbles on the upper surface of the aluminum liquid.
  • Refining agent refining treatment of Al-Ti-B master alloy
  • Aluminum-titanium-boron master alloy purchased from Nantong Angshen Metal Materials Co., Ltd. (composition and content: Ti: 5%, B: 1%, the rest: Al)
  • Pretreatment Use a grinder to clean the oxide skin and surface layer on the surface of the high-purity aluminum ingot.
  • Ultrasonic cleaning Put the pretreated high-purity aluminum ingot into the cleaning agent for ultrasonic treatment.
  • Drying Put the high-purity aluminum ingot after ultrasonic cleaning into an oven and bake at 60-100°C for 30-60 minutes.
  • Refining treatment is performed after the high-purity aluminum is melted. Specifically: Refining the molten high-purity aluminum through the Ar+graphite automatic degassing stirring rod. Refining by blowing Ar at 740-760°C for 5-10 minutes, the amount of refining being blown in is 0.1-0.3% of the melt, and kept for 3-5 minutes. After that, let it stand for 10-20 minutes, put 0.1-0.3% scum remover in it to make it evenly disperse, and remove the scum on the surface.
  • Refining treatment The whole process is under the protection of argon atmosphere, and the refining treatment is performed after the rare earth aluminum-lanthanum alloy is melted. Feed the Ar+graphite automatic degassing stirring rod to refine the melted one. Refining with Ar blowing at 760-780°C for 5-10 minutes, the amount of refining being blown in is 0.1-0.3% of the melt, and kept at 3-5 minutes. During the refining process, there should be no boiling bubbles on the upper surface of the aluminum liquid. Remove scum on the surface of the melt: put in 0.1-0.3% slag remover in 15-20 minutes and spread evenly to remove the scum on the surface.
  • the aluminum melt, the rare earth aluminum alloy, the aluminum-strontium master alloy, and the aluminum-titanium-boron master alloy are respectively prepared through the above, and then mixed and smelted to obtain a composite rare earth alloy.
  • the rare earth aluminum alloy is firstly added to the aluminum melt, then the aluminum strontium alloy is added, and finally the aluminum titanium boron alloy is added. details as follows:
  • Step 1 Ingredients: Preheat the high-purity aluminum, aluminum-titanium-boron master alloy, aluminum-strontium master alloy, and rare earth aluminum alloy obtained above according to the required mass percentage.
  • high-purity aluminum 4.8 parts
  • aluminum-titanium-boron master alloy 0.2 parts
  • aluminum-strontium master alloy 60 parts
  • rare earth aluminum alloy 35 parts.
  • Step 2 Adding and melting the rare earth aluminum alloy: For the above aluminum melt, first heat the above purified rare earth aluminum alloy to 780-820°C to soften before melting, and then control the overall temperature of the aluminum melt at 760-820°C 780°C, add rare earth aluminum alloy into the aluminum melt for heat preservation.
  • the whole process adopts the protection of argon atmosphere and melts the rare earth aluminum alloy.
  • Step 3 After the rare earth aluminum alloy is completely melted, the temperature is controlled at 750-770° C. and stirred for 5-10 minutes.
  • the whole process is protected by an argon atmosphere, and the stirring rod is made of graphite material and preheated to 400-500°C before stirring.
  • Step 4 heat-preserve the melted melt at 740-760° C. and control the heat-retaining time within 5-20 minutes. In this stage, an alloying reaction occurs.
  • Step 5 After the heat preservation is completed, refining, degassing and slag removal are carried out. 0.3% refining agent is blown into the melt by argon, and the aeration time is controlled at 3 to 8 minutes; after that, further add 0.2% slag remover, stir for 5 minutes and let stand to remove the slag and impurities on the surface of the melt . The whole process is protected by argon atmosphere.
  • the aluminum melt is sampled before and during refining and its density is determined to estimate the hydrogen content.
  • the measurement method adopts the density method (compared with the theoretical value of aluminum of 2.70g/cm3), the closer the measured sample is to 2.7g/cm3, the lower the internal hydrogen content of aluminum. Generally, it cannot reach 2.7g/cm3 normally; the density test of the sample is about 2.65g/cm3 to estimate the hydrogen content.
  • the hydrogen content must be vacuumized. The slag agent is refined again.
  • Step 6 Stand still: put the melt that has been added with the rare earth aluminum alloy and refined for 3-5 minutes, and the temperature is controlled at 740-760 degrees.
  • Step 7 Adding and melting the aluminum-strontium master alloy: adding the above-mentioned refined aluminum-strontium master alloy into the melt in step 6, and controlling the temperature at 780-820° C. to completely melt the aluminum-strontium master alloy. The whole process is protected by argon atmosphere, and the aluminum-strontium master alloy is melted.
  • Step 8 After the aluminum-strontium master alloy is melted, control the temperature at 740-760° C. and stir for 3-8 minutes to achieve homogenization. The whole process is protected by argon atmosphere, the stirring rod is made of graphite material, and it is preheated to 400-500°C before stirring.
  • Step 9 heat preservation treatment is carried out at 725-750°C.
  • the heat preservation time is controlled at 15-30 minutes.
  • Step 10 Refining, degassing and slag removal: After the heat preservation of the melt is completed, blow in 0.3% of the refining agent into the aluminum-rare-earth composite melt after argon gas is introduced, and the ventilation time is controlled at 5 to 10 minutes; put in 0.2% of Put the slag removal agent into the aluminum melt, stir for 5 minutes and remove the slag and impurities on the surface of the aluminum-rare-earth composite melt. The whole process is protected by argon atmosphere.
  • the aluminum melt is sampled before and during refining to determine the hydrogen content. (Hydrogen content requirement: greater than or equal to 2.65g/cm 3 ;) During the hydrogen measurement process, it must be vacuumized. If the hydrogen content is unqualified, then further refining, that is, adding refining agents and slag removers to refine again.
  • Step 11 Add Al-Ti-B master alloy: Add Al-Ti-B master alloy to the melt treated in Step 10 above, heat to melt completely, and stir evenly for 3-5 minutes to homogenize.
  • Step 12 heat preservation: after stirring, heat the melt for 8-12 minutes, and control the temperature at 715-725°C.
  • Step 13 Refining, degassing and slag removal: After the heat preservation of the melt is completed, blow in 0.3% of the refining agent into the aluminum-rare-earth composite melt after argon gas is introduced, and the ventilation time is controlled at 5 to 10 minutes; put in 0.2% of Put the slag removal agent into the aluminum melt, stir for 5 minutes and remove the slag and impurities on the surface of the aluminum-rare-earth composite melt. The whole process is protected by argon atmosphere.
  • the aluminum melt is sampled before and during refining to determine the hydrogen content. (Hydrogen content requirement: greater than or equal to 2.65g/cm 3 ;) Vacuum treatment must be performed during the hydrogen measurement process. If the hydrogen content is unqualified, further refining is carried out, that is, refining agents and slag removers are added repeatedly until it is qualified.
  • Step 14 casting: the mold is preheated at 300-400°C.
  • the temperature of the composite rare earth alloy melt obtained in step 13 above is controlled at 715-725° C. for casting.
  • the oxides on the surface of the aluminum-rare-earth composite melt are filtered through a glass fiber filter; before each casting, the surface of the aluminum-rare-earth composite melt is filtered before casting.
  • the cooling control of the casting mold adopts a water cooling method to cool the aluminum-rare-earth composite melt cast into the mold.
  • the solidification speed of the aluminum melt is controlled at 50-100°C/s, and the solidification method is sequential solidification.
  • composition ratio of the composite rare earth aluminum alloy is not limited by the above embodiments, for example, it can be designed such that the mass ratio of the rare earth metal: strontium: titanium or titanium boron weight is 1: (0.1-1.2): (0.1-1.2).
  • the aluminum-silicon-magnesium alloy, the composite rare-earth aluminum alloy, and the aluminum-titanium-boron master alloy are prepared with a mass ratio of aluminum alloy:composite rare earth aluminum alloy:aluminium-titanium-boron master alloy of 99.4:0.4:0.2.
  • Heat preservation After stirring, control the temperature at 735 degrees for heat preservation, and the heat preservation time is controlled at 20 minutes;
  • Add refiner add 0.2% Al-Ti-B intermediate alloy to the refined aluminum water, wait for it to melt and stir and continue refining;
  • Heat preservation and standing After refining, the aluminum water flows into the heat preservation pool, and when the temperature is controlled at 710 ⁇ 3 degrees, the slag and impurities on the surface of the aluminum water are removed after standing for 10 ⁇ 2 minutes;
  • the refined modified aluminum alloy with the above temperature controlled at 700 ⁇ 5 is cast into the mold, and the modified aluminum alloy biscuit is obtained after cooling.
  • the thickness of the modified aluminum alloy biscuit is 30mm.
  • Solution treatment put the modified aluminum alloy biscuit in a heating furnace, heat it to 540°C at a heating rate of 2°C/min, and keep it there for 120min.
  • the modified aluminum alloy biscuit after the above solid solution treatment is added into a circulating water bath at a temperature of 65° C., and water is quenched for 3 minutes.
  • Fig. 1 shows the metallographic structure images of aluminum alloy parts in different stages, wherein, (a) is the image of A356 aluminum alloy before heat treatment, (b) is the image of A356 aluminum alloy after heat treatment, (c) is the The image after compound modification and before heat treatment in Example 1, (d) is the image after compound modification and heat treatment in Example 1.
  • the metallographic structure of the modified and heat-treated aluminum alloy in this embodiment is further increased compared with the rounded spherical ⁇ -Al phase, and the primary ⁇ -Al phase and dendrites are basically invisible. That is to say, the grains are further homogenized and the microstructure is more uniform.
  • the spherical ⁇ -Al phase is uniformly distributed at the grain boundaries.
  • the metallographic structure of the aluminum alloy after heat treatment ie (c)
  • the primary ⁇ -Al phase and dendrites are basically invisible. That is to say, the grains are further homogenized and the microstructure is more uniform.
  • Example 1 Through the heat treatment in Example 1, even without heat treatment, the plasticity can be greatly improved.
  • its yield strength and tensile strength are greatly improved (compared to the unmodified and unheated aluminum alloy master ingot, the yield strength and tensile strength are increased by nearly 3 times respectively , more than 2 times), while maintaining a high level of elongation (compared to the untreated aluminum alloy master ingot, it has increased by more than 5 times), which greatly improves the comprehensive mechanical properties.
  • rare earth aluminum alloy (the purification treatment of rare earth aluminum alloy is the same as in Example 1): aluminum strontium alloy: aluminum titanium boron intermediate alloy mass ratio is the ratio of 99.4:0.2:0.2:0.2 to prepare the above-mentioned aluminum silicon magnesium alloy, rare earth Aluminum alloys, aluminum-strontium master alloys, and aluminum-titanium-boron master alloys.
  • Heat preservation After stirring, control the temperature at 735 degrees for heat preservation, and the heat preservation time is controlled at 20 minutes;
  • Add aluminum-strontium master alloy add 0.2% aluminum-strontium master alloy to the refined aluminum water, wait for it to melt and stir and continue refining;
  • Heat preservation Next, heat preservation treatment is carried out at 725-750°C, and the heat preservation time is controlled at 15-30 minutes;
  • Add refiner add 0.2% Al-Ti-B intermediate alloy to the refined aluminum water, wait for it to melt and stir and continue refining;
  • Heat preservation and standing After refining, the aluminum water flows into the heat preservation pool, and when the temperature is controlled at 710 ⁇ 3 degrees, the slag and impurities on the surface of the aluminum water are removed after standing for 10 ⁇ 2 minutes;
  • the modified alloy 2 represents the green body after modification without heat treatment.
  • the rare earth aluminum alloy and the aluminum strontium master alloy are first smelted to prepare a composite rare earth aluminum alloy, and the composite modified aluminum alloy obtained by modifying the composite rare earth aluminum alloy is Part (i.e. embodiment 1) has higher comprehensive mechanical properties.
  • Example 1 For specific preparation, refer to Example 1, and its detailed description is omitted here.
  • Example 3 It can be seen from Table 3 that the heat treatment in Example 3 can also obtain similar results to those in Examples 1 and 2 above. That is to say, the preparation process of the present invention is also applicable to the eutectic aluminum alloy, which can obtain better strength and higher toughness.

Abstract

Provided are a high-plasticity composite modified aluminum alloy part and a preparation method therefor. The preparation method comprises the following steps: step S1, providing an aluminum alloy melt; step S2, providing a modifier; step S3, adding the modifier into the aluminum alloy melt under an inert gas atmosphere and smelting same to obtain a modified aluminum alloy melt; step S4, performing casting by using the modified aluminum alloy melt to obtain the cast aluminum alloy blank; and S5, performing a heat treatment on the modified aluminum alloy blank, wherein the heat treatment comprises: a solution treatment, involving heating the aluminum alloy blank to 530ºC-550ºC, and maintaining the temperature for 120-300 min; a water quenching treatment, involving adding the aluminum alloy blank after the solution treatment into a water bath with the temperature of 60ºC-70ºC, and water quenching same for 2-4 min; an aging treatment, involving maintaining the aluminum alloy blank after the water quenching treatment at 110ºC-140ºC for 120-240 min, then further raising the temperature to 160ºC-200ºC and maintaining the temperature for 20-60 min, and then cooling to room temperature to obtain the high-plasticity composite modified aluminum alloy part.

Description

高塑性复合改性铝合金制件及其制备方法High-plastic composite modified aluminum alloy parts and preparation method thereof 技术领域technical field
本发明涉及合金材料及制备技术领域，具体涉及一种高塑性复合改性铝合金制件及其制备方法。The invention relates to the technical field of alloy materials and preparation, in particular to a high-plastic composite modified aluminum alloy product and a preparation method thereof.
背景技术Background technique
铝合金是工业中应用最广泛的一类有色金属结构材料，在航空、航天、汽车、机械制造、船舶及化学工业中已大量应用。铸造铝合金具有铸造流动性、气密性好、收缩率小及热裂倾向小等特点，它成为汽车轮毂轻量化的首选材料。Aluminum alloy is the most widely used non-ferrous metal structural material in industry, and has been widely used in aviation, aerospace, automobile, machinery manufacturing, shipbuilding and chemical industry. Cast aluminum alloy has the characteristics of casting fluidity, good air tightness, small shrinkage rate and small thermal cracking tendency, etc., and it has become the first choice material for lightweight automobile wheels.
然而，人们对铝合金的要求也越来越高，不仅要保持原有的轻质的特点，同时还要具有一定的强度，尤其是在汽车零部件和工业的生产上。此外，铝合金车轮零部件需要中等强度更高的塑韧性，以避免车轮在发生正撞冲击和侧撞冲击时(在设计载荷承受范围内)导致瞬间断裂。However, people's requirements for aluminum alloys are getting higher and higher, not only to maintain the original lightweight characteristics, but also to have a certain strength, especially in the production of auto parts and industries. In addition, aluminum alloy wheel parts require medium strength and higher ductility to avoid instantaneous fracture of the wheel in the event of frontal impact and side impact (within the design load bearing range).
为此，提出了利用变质剂例如铝锶合金对其进行改质，同时结合细化剂对其进行细化的工艺。然而，传统的改性仍然不能得到理想的强度与塑性。在此基础上，展开了对于铸造铝合金进行热处理的研究。但是，由于铝合金零部件的成分差异，热处理的步骤也不同，目前的热处理需要高的温度，耗能大，时间长，增加处理成本，且由于直接采用较高温度进行处理，不利于各相态的相互转化和脱溶的均匀进行，造成合金机械性能的不均匀。For this reason, a process of modifying it with a modifier such as aluminum-strontium alloy and refining it with a refiner is proposed. However, the traditional modification still cannot obtain ideal strength and plasticity. On this basis, the research on heat treatment of cast aluminum alloy is carried out. However, due to the difference in the composition of aluminum alloy parts, the steps of heat treatment are also different. The current heat treatment requires high temperature, consumes a lot of energy, takes a long time, and increases the processing cost. The mutual transformation of the state and the uniform progress of the precipitation cause the uneven mechanical properties of the alloy.
为此，亟需提供一种能够进一步提高铝合金制件的塑性以及机械强度的制备工艺。Therefore, there is an urgent need to provide a preparation process that can further improve the plasticity and mechanical strength of aluminum alloy parts.
发明内容Contents of the invention
有鉴于此，本发明提供一种能够进一步提高铝合金的塑性及机械强度的高塑性复合改性铝合金制件及其制备方法。In view of this, the present invention provides a high-plastic composite modified aluminum alloy product and a preparation method thereof, which can further improve the plasticity and mechanical strength of the aluminum alloy.
为解决上述技术问题，本发明采用以下技术方案：In order to solve the problems of the technologies described above, the present invention adopts the following technical solutions:
根据本发明第一方面实施例的高塑性复合改性铝合金制件的制备方法，包括如下步骤：The method for preparing a high-plastic composite modified aluminum alloy product according to the embodiment of the first aspect of the present invention includes the following steps:
步骤S1，提供铝合金熔体；Step S1, providing an aluminum alloy melt;
步骤S2，提供改性剂；Step S2, providing a modifier;
其中，所述改性剂为稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金的组合，Wherein, the modifier is a combination of rare earth aluminum alloy, aluminum-strontium master alloy, aluminum-titanium or aluminum-titanium-boron master alloy,
或者所述改性剂为复合稀土铝合金、铝钛或铝钛硼中间合金的组合，所述复合稀土铝合金中含有锶、钛或钛硼、以及稀土金属，Or the modifier is a combination of composite rare earth aluminum alloy, aluminum titanium or aluminum titanium boron intermediate alloy, and the composite rare earth aluminum alloy contains strontium, titanium or titanium boron, and rare earth metals,
所述稀土铝合金、所述复合稀土铝合金中的稀土金属为镧、铈、钇中的任意一种或多种；The rare earth metal in the rare earth aluminum alloy and the composite rare earth aluminum alloy is any one or more of lanthanum, cerium, and yttrium;
步骤S3，在惰性气体气氛下，在所述铝合金熔体中，加入所述改性剂并熔炼，得到改性铝合金熔体；Step S3, adding the modifying agent to the aluminum alloy melt under an inert gas atmosphere and melting to obtain a modified aluminum alloy melt;
步骤S4，利用所述改性铝合金熔体进行浇铸，得到所述铸造铝合金素坯；Step S4, using the modified aluminum alloy melt to perform casting to obtain the cast aluminum alloy biscuit;
步骤S5，对所述铝合金素坯进行热处理，其中，所述热处理包括：Step S5, performing heat treatment on the aluminum alloy green body, wherein the heat treatment includes:
固溶处理，将所述铝合金素坯加热至530-550℃，并保温120-300min；Solution treatment, heating the aluminum alloy biscuit to 530-550°C and keeping it warm for 120-300min;
淬水处理，将经过固溶处理后的铝合金素坯加入温度为60-70℃的水浴中，淬水2-4min；Water quenching treatment, adding the aluminum alloy biscuit after solid solution treatment into a water bath at a temperature of 60-70°C, and quenching water for 2-4 minutes;
时效处理，将经过淬水处理后的铝合金素坯在110-140℃保温120-240min，此后进一步升温至160-200℃并保温20-60min，此后冷却至室温，得到所述高塑性复合改性铝合金制件。For aging treatment, heat the quenched aluminum alloy biscuit at 110-140°C for 120-240 minutes, then further raise the temperature to 160-200°C and hold it for 20-60 minutes, and then cool it to room temperature to obtain the high-plastic composite modification. High-strength aluminum alloy parts.
进一步地，所述步骤S1包括：Further, the step S1 includes:
提供铝合金母锭；Provide aluminum alloy master ingot;
去除所述铝合金母锭的表面氧化皮层并进行清洗、烘干；removing the oxide skin layer on the surface of the aluminum alloy master ingot, cleaning and drying;
将烘干后的铝合金母锭进行熔炼，并进行精炼、除渣，得到所述铝合金熔体，Melting the dried aluminum alloy mother ingot, refining and removing slag to obtain the aluminum alloy melt,
其中，所述铝合金母锭的成分为亚共晶铝合金或共晶铝合金。Wherein, the composition of the aluminum alloy master ingot is hypoeutectic aluminum alloy or eutectic aluminum alloy.
根据本发明的一些实施例，所述改性剂为稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金的组合，其中，所述铝锶中间合金与所述铝钛或铝钛硼中间合金间隔开加入，According to some embodiments of the present invention, the modifier is a combination of rare earth aluminum alloy, aluminum-strontium master alloy, aluminum-titanium or aluminum-titanium-boron master alloy, wherein the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium The boron master alloy is added at intervals,
所述稀土铝合金最先加入，或者与首先加入的一方一同加入，或者在所述铝锶中间合金与所述铝钛或铝钛硼中间合金加入间隙加入。The rare earth aluminum alloy is added first, or added together with the first added party, or added between the addition of the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy.
进一步地，所述步骤S3包括：Further, the step S3 includes:
步骤S301，在所述铝合金熔体中加入所述稀土铝合金并进行熔炼，得到第一均匀混合熔体；Step S301, adding the rare earth aluminum alloy into the aluminum alloy melt and melting to obtain a first homogeneously mixed melt;
步骤S302，在所述第一均匀混合熔体中加入所述铝锶中间合金并继续熔炼，得到第二均匀混合熔体；Step S302, adding the aluminum-strontium master alloy into the first homogeneously mixed melt and continuing to smelt to obtain a second homogeneously mixed melt;
步骤S303，在所述第二均匀混合熔体中加入所述铝钛或铝钛硼中间合金并继续熔炼，得到所述改性铝合金。Step S303, adding the aluminum-titanium or aluminum-titanium-boron master alloy into the second homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
根据本发明的另一些实施例，所述改性剂为复合稀土铝合金、铝钛或铝钛硼中间合金的组合，所述步骤S3包括：According to other embodiments of the present invention, the modifying agent is a combination of composite rare earth aluminum alloy, aluminum titanium or aluminum titanium boron master alloy, and the step S3 includes:
步骤S310，在所述铝合金熔体中加入所述复合稀土铝合金并进行熔炼，得到第四均匀混合熔体；Step S310, adding the composite rare earth aluminum alloy into the aluminum alloy melt and melting to obtain a fourth uniformly mixed melt;
步骤S320，在所述第四均匀混合熔体中加入所述铝钛或铝钛硼中间合金并继续熔炼，得到所述改性铝合金。Step S320, adding the aluminum-titanium or aluminum-titanium-boron master alloy into the fourth homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
进一步地，所述复合稀土铝合金的制备包括：Further, the preparation of the composite rare earth aluminum alloy includes:
步骤S211，提供所述铝熔体；Step S211, providing the aluminum melt;
步骤S212，提供铝锶中间合金、铝钛或铝钛硼中间合金、以及稀土铝中间合金，所述稀土铝中间合金中的稀土金属为选自镧、铈、钇中的一种或多种；Step S212, providing an aluminum-strontium master alloy, an aluminum-titanium or aluminum-titanium-boron master alloy, and a rare earth aluminum master alloy, wherein the rare earth metal in the rare earth aluminum master alloy is one or more selected from lanthanum, cerium, and yttrium;
步骤S213，在惰性气体气氛下，在所述铝熔体中，依次加入所述稀土铝中间合金、铝锶中间合金、铝钛或铝钛硼中间合金并熔炼，得到所述复合稀土合金。Step S213, under an inert gas atmosphere, sequentially add the rare earth aluminum master alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy into the aluminum melt and melt to obtain the composite rare earth alloy.
进一步地，所述改性剂占所述改性铝合金熔体总量的0.4-0.6wt％，所述稀土金属：锶：钛或钛硼总量的质量比为1:(0.1-1.2)：(0.1-1.2)。Further, the modifier accounts for 0.4-0.6wt% of the total amount of the modified aluminum alloy melt, and the mass ratio of the rare earth metal: strontium: titanium or the total amount of titanium boron is 1: (0.1-1.2) : (0.1-1.2).
进一步地，所述步骤S5中，所述固溶处理中的升温速率控制在1.5-3℃/min，保温时间控制在120-180min。Further, in the step S5, the heating rate in the solution treatment is controlled at 1.5-3° C./min, and the holding time is controlled at 120-180 min.
进一步地，所述固溶处理、所述淬水处理、以及所述时效处理为连续处理，且所述水浴为循环水浴，所述淬水处理后，在进行所述时效处理前所述铸造铝合金素坯的温度保持在55℃以上。Further, the solid solution treatment, the quenching treatment, and the aging treatment are continuous treatments, and the water bath is a circulating water bath. After the quenching treatment, before the aging treatment, the cast aluminum The temperature of the alloy green body is kept above 55°C.
进一步地，所述时效处理阶段，从110-140℃以2-4℃/min的升温速率升温至160-200℃，此后自然冷却至室温。Further, in the aging treatment stage, the temperature is raised from 110-140°C to 160-200°C at a heating rate of 2-4°C/min, and then naturally cooled to room temperature.
根据本发明第二方面实施例的高塑性复合改性铝合金制件，由根据上述任一实施例所述的制备方法制备得到，所述高塑性复合改性铝合金制件的抗拉强度为280MPa以上，屈服强度为200MPa以上，延伸率为12％以上。The high-plastic composite modified aluminum alloy product according to the second aspect of the present invention is prepared by the preparation method described in any of the above-mentioned embodiments, and the tensile strength of the high-plastic composite modified aluminum alloy product is: 280MPa or more, the yield strength is 200MPa or more, and the elongation is 12% or more.
本发明的上述技术方案至少具有如下有益效果之一：The technical solution of the present invention has at least one of the following beneficial effects:
根据本发明实施例的高塑性复合改性铝合金制件的制备方法，通过引入稀土金属对铝合金进行改质，并结合特定的热处理工艺对铸造件进行处理，能够大幅提高其塑性(延伸率)，减少脆裂等发生，同时提高其机械强度以满足航空、航天、汽车领域等需求。According to the preparation method of high-plastic composite modified aluminum alloy parts in the embodiment of the present invention, the aluminum alloy is modified by introducing rare earth metals, and the casting is treated in combination with a specific heat treatment process, so that its plasticity (elongation rate) can be greatly improved ), reduce the occurrence of brittle cracks, and at the same time improve its mechanical strength to meet the needs of aviation, aerospace, and automotive fields.
附图说明Description of drawings
图1为不同阶段铝合金制件的金相组织图像，其中，(a)为热处理前的A356铝合金的图像，(b)为热处理后的A356铝合金的图像，(c)为实施例1中复合改性后、热处理前的图像，(d)为实施例1的复合改性并进行热处理后的图像。Fig. 1 is the metallographic structure image of aluminum alloy parts in different stages, wherein, (a) is the image of A356 aluminum alloy before heat treatment, (b) is the image of A356 aluminum alloy after heat treatment, (c) is embodiment 1 In (d) is the image after compound modification and heat treatment in Example 1.
具体实施方式Detailed ways
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例对本发明的技术方案进行清楚、完整地描述。显然，所描述的实施例是本发明的一部分实施例，而不是全部的实施例。基于所描述的本发明的实施例，本领域普通技术人员所获得的所有其他实施例，都属于本发明保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Apparently, the described embodiments are some, not all, embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the described embodiments of the present invention belong to the protection scope of the present invention.
除非另作定义，本发明中使用的技术术语或者科学术语应当为本发明所属领域内具有一般技能的人士所理解的通常意义。本发明中使用的“第一”、“第二”以及类似的词语并不表示任何顺序、数量或者重要性，而只是用来区分不同的组成部分。同样，“一个”或者“一”等类似词语也不表示数量限制，而是表示存在至少一个。Unless otherwise defined, the technical terms or scientific terms used in the present invention shall have the usual meanings understood by those skilled in the art to which the present invention belongs. "First", "second" and similar words used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. Likewise, words like "a" or "one" do not denote a limitation in quantity, but indicate that there is at least one.
下面首先结合具体描述根据本发明实施例的高强度复合改性铝合金制件的制备方法。The method for preparing a high-strength composite modified aluminum alloy product according to an embodiment of the present invention will first be described in detail below.
根据本发明实施例的高塑性复合改性铝合金制件的制备方法，包括如下步骤：The method for preparing a high-plastic composite modified aluminum alloy product according to an embodiment of the present invention includes the following steps:
步骤S1，提供铝合金熔体。Step S1, providing an aluminum alloy melt.
也就是说，首先准备铝合金熔体。That is, first, an aluminum alloy melt is prepared.
在此，需要说明的是，可以采用市售的高纯铝合金锭直接加热熔化制备铝合金熔体，也可以对铝合金锭进行进一步纯化。纯化处理例如可以包括如下步骤：Here, it should be noted that a commercially available high-purity aluminum alloy ingot can be directly heated and melted to prepare an aluminum alloy melt, or the aluminum alloy ingot can be further purified. Purification treatment may include the following steps, for example:
步骤S11，提供铝合金锭；Step S11, providing an aluminum alloy ingot;
步骤S12，去除所述铝合金锭表面的氧化皮层；Step S12, removing the oxide layer on the surface of the aluminum alloy ingot;
步骤S13，对去除所述氧化皮层的铝合金锭进行清洗，烘干；Step S13, cleaning and drying the aluminum alloy ingot from which the scale layer has been removed;
步骤S14，将烘干后的所述铝合金锭进行熔炼，得到初始熔体；Step S14, melting the dried aluminum alloy ingot to obtain an initial melt;
步骤S15，对所述初始熔体进行精炼，得到所述铝合金熔体。Step S15, refining the initial melt to obtain the aluminum alloy melt.
也就是说，对于铝合金锭，首先去除其表面的氧化皮层，此后进行清洗以去除表面浮屑，烘干后进行熔炼，并对熔体进行精炼。关于具体的精炼处理过程后面进行详细述说。That is to say, for aluminum alloy ingots, the oxide scale layer on the surface is first removed, then cleaned to remove surface scum, smelted after drying, and the melt is refined. The specific refining process will be described in detail later.
经过上述纯化处理后，能够去除掉其中不希望存在的杂质，例如Fe、氧化物、等等。有利于进一步提高稀土合金的变质与细化作用。After the above purification treatment, undesired impurities such as Fe, oxides, etc. can be removed. It is beneficial to further improve the modification and refinement of rare earth alloys.
在此需要补充说明的是，关于其中的Fe及其氧化物，例如可以通过添加锰或铝锰合金，以形成表面浮渣来去除。It should be added here that Fe and its oxides can be removed by adding manganese or aluminum-manganese alloy to form surface scum, for example.
作为被改性的母体，即铝合金熔体，例如可以是铝镁合金、铝硅合金、铝硅镁合金等，本发明对此不作具体限制。As the matrix to be modified, that is, the aluminum alloy melt, for example, it may be an aluminum-magnesium alloy, an aluminum-silicon alloy, an aluminum-silicon-magnesium alloy, etc., which is not specifically limited in the present invention.
步骤S2，提供改性剂。Step S2, providing a modifier.
其中，所述改性剂为稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金的组合，或者所述改性剂为复合稀土铝合金、铝钛或铝钛硼中间合金的组合，Wherein, the modifier is a combination of rare earth aluminum alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy, or the modifier is a combination of compound rare earth aluminum alloy, aluminum titanium or aluminum titanium boron master alloy ,
所述复合稀土铝合金中含有锶、钛或钛硼、以及稀土金属，The composite rare earth aluminum alloy contains strontium, titanium or titanium boron, and rare earth metals,
所述稀土铝合金、所述复合稀土铝合金中的稀土金属为镧、铈、钇中的任意一种或多种。The rare earth metal in the rare earth aluminum alloy and the composite rare earth aluminum alloy is any one or more of lanthanum, cerium, and yttrium.
也就是说，存在如下两种实施方式：That is to say, there are two implementation modes as follows:
实施方式一：Implementation mode one:
所述改性剂为稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金的组合。The modifier is a combination of rare earth aluminum alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy.
其中，所述铝锶中间合金即变质剂，所述铝钛中间合金或铝钛硼中间合金即细化剂。也就是说，可以使用常规的变质剂和细化剂。Wherein, the aluminum-strontium master alloy is the modifier, and the aluminum-titanium master alloy or the aluminum-titanium-boron master alloy is the refiner. That is, conventional modifiers and refiners can be used.
进一步地，对于所述变质剂和/或所述细化剂，可以采用市售的材料，也可以通过分别称取相应的金属锶、钛、钛&硼，将其熔化在铝熔体中形成均匀的合金制备得到。Further, for the modifier and/or the refiner, commercially available materials can be used, or the corresponding metal strontium, titanium, titanium & boron can be weighed and melted in aluminum melt to form A homogeneous alloy is prepared.
另外，在常规的变质剂和细化剂之外，进一步引入稀土铝合金，以克服由于变质剂和细化剂之间的“中毒”反应导致的机械性能的限制。作为稀土铝合金中的稀土金属，考虑到变质剂中的锶以及细化剂中的钛、硼，可以选择电子结构介于其间的IIIB族元素。综合考虑其稳定性、资源等，优选地，采用钇、镧系金属中的镧、铈中的一种或多种。稀土铝合金例如可以采用市售的Al-10Ce、Al-20Ce、Al-20La、Al-10La、Al-20Y、Al-10Y中一种或多种。In addition, in addition to conventional modifiers and refiners, rare earth aluminum alloys are further introduced to overcome the limitation of mechanical properties due to the "poisoning" reaction between modifiers and refiners. As the rare earth metal in the rare earth aluminum alloy, considering the strontium in the modifier and the titanium and boron in the refiner, the group IIIB elements whose electronic structure is in between can be selected. In comprehensive consideration of its stability, resources, etc., preferably, one or more of yttrium, lanthanum in lanthanide metals, and cerium are used. As the rare earth aluminum alloy, for example, one or more of commercially available Al-10Ce, Al-20Ce, Al-20La, Al-10La, Al-20Y, and Al-10Y can be used.
另外，也可以自行制备稀土铝合金，例如可以采用下述方法制备得到：In addition, the rare earth aluminum alloy can also be prepared by itself, for example, it can be prepared by the following method:
在惰性气氛下在所述铝熔体其中加入所述稀土金属或含所述稀土金属的中间合金，加热的同时搅拌至完全熔化；Adding the rare earth metal or the master alloy containing the rare earth metal into the aluminum melt under an inert atmosphere, stirring while heating until completely melted;
待完全熔化后继续保温10-20分钟使其均质化；After it is completely melted, keep warm for 10-20 minutes to make it homogenized;
对均质化熔体进行精炼；Refining the homogenized melt;
精炼后静置预定时间，并进行浇注，得到所述稀土铝合金。After refining, the rare earth aluminum alloy is obtained by standing for a predetermined time and pouring.
其中，铝熔体可以采用市售的高纯铝锭参考上述对铝合金锭的纯化处理进行相应的处理，在此不再进行赘述。Wherein, the aluminum melt can be treated by using commercially available high-purity aluminum ingots with reference to the above-mentioned purification treatment of aluminum alloy ingots, which will not be repeated here.
此外，对于市售的铝锶中间合金，铝钛中间合金或铝钛硼中间合金，稀土铝合金，可以分别依次进行去氧化皮层、超声清洗、精炼处理。由此，能够进一步去除其中不希望的杂质、氧化物，有利于提高作为产品的复合稀土合金的细化和变质作用。In addition, for commercially available aluminum-strontium master alloys, aluminum-titanium master alloys or aluminum-titanium-boron master alloys, and rare-earth aluminum alloys, descaling, ultrasonic cleaning, and refining can be performed sequentially, respectively. In this way, unwanted impurities and oxides can be further removed, which is beneficial to improving the refinement and modification of the composite rare earth alloy as a product.
实施方式二：Implementation mode two:
所述改性剂为复合稀土铝合金、铝钛或铝钛硼中间合金的组合。The modifier is a combination of composite rare earth aluminum alloy, aluminum titanium or aluminum titanium boron master alloy.
作为复合稀土铝合金，可以利用上述稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金、以及铝熔体经熔炼、精炼制备得到。The composite rare earth aluminum alloy can be prepared by melting and refining the above rare earth aluminum alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy, and aluminum melt.
例如，所述复合稀土铝合金的制备可以包括：For example, the preparation of the complex rare earth aluminum alloy may include:
步骤S211，提供铝熔体；Step S211, providing aluminum melt;
步骤S212，提供铝锶中间合金、铝钛或铝钛硼中间合金、以及稀土铝合金，所述稀土铝合金中的稀土金属为选自镧、铈、钇中的一种或多种；Step S212, providing an aluminum-strontium master alloy, an aluminum-titanium or aluminum-titanium-boron master alloy, and a rare earth aluminum alloy, wherein the rare earth metal in the rare earth aluminum alloy is one or more selected from lanthanum, cerium, and yttrium;
步骤S213，在惰性气体气氛下，在所述铝熔体中，加入所述稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金并熔炼，得到所述复合稀土合金。Step S213, adding the rare earth aluminum alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy into the aluminum melt under an inert gas atmosphere and melting to obtain the composite rare earth alloy.
其中，所述铝锶中间合金与所述铝钛或铝钛硼中间合金间隔开加入，所述稀土铝合金在所述铝锶中间合金与所述铝钛或铝钛硼中间合金之前加入，或者与首先加入的一方一同加入，或者在所述铝锶中间合金与所述铝钛或铝钛硼中间合金加入间隙加入。Wherein, the aluminum-strontium master alloy is added separately from the aluminum-titanium or aluminum-titanium-boron master alloy, and the rare earth aluminum alloy is added before the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy, or It is added together with the first addition, or added between the addition of the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy.
优选地，在所述铝熔体中依次间隔开加入所述稀土铝合金、所述铝锶中间合金、所述铝钛或铝钛硼中间合金。Preferably, the rare earth aluminum alloy, the aluminum-strontium master alloy, the aluminum-titanium or aluminum-titanium-boron master alloy are sequentially added to the aluminum melt at intervals.
步骤S3，在惰性气体气氛下，在所述铝合金熔体中，加入所述改性剂并熔炼，得到所述改性铝合金熔体。In step S3, under an inert gas atmosphere, the modifier is added to the aluminum alloy melt and smelted to obtain the modified aluminum alloy melt.
也就是说，在准备好铝熔体、改性剂之后，在惰性气体气氛下，将改性剂加入到铝熔体中进一步熔炼，得到改性铝合金熔体。That is to say, after the aluminum melt and the modifier are prepared, the modifier is added to the aluminum melt for further melting under an inert gas atmosphere to obtain a modified aluminum alloy melt.
根据本发明实施例的制备方法，通过在改性剂中引入稀土金属，极大地克服了变质剂与细化剂之间的相互毒化作用，可以提高变质剂和细化剂的添加量，同时能够提高变质和细化的效果。According to the preparation method of the embodiment of the present invention, by introducing rare earth metals into the modifying agent, the mutual poisoning effect between the modifying agent and the refining agent can be greatly overcome, the addition amount of modifying agent and refining agent can be increased, and at the same time it can Improves the effect of metamorphism and refinement.
针对上述两种组合的改性剂，分别进行如下熔炼。For the modifiers of the above two combinations, the following smelting was carried out respectively.
针对所述改性剂为稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金的组合：For the combination of the modifier being a rare earth aluminum alloy, an aluminum strontium master alloy, an aluminum titanium or an aluminum titanium boron master alloy:
具体地，各稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金及其预处理可以参考上述步骤S2。Specifically, for each rare earth aluminum alloy, aluminum-strontium master alloy, aluminum-titanium or aluminum-titanium-boron master alloy and its pretreatment, reference may be made to the above step S2.
在该组合的情况下，其中，所述铝锶中间合金与所述铝钛或铝钛硼中间合金间隔开加入，所述稀土铝合金最先加入，或者与首先加入的一方一同加入，或者在所述铝锶中间合金与所述铝钛或铝钛硼中间合金加入间隙加入。In the case of this combination, wherein the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy are added at intervals, the rare earth aluminum alloy is added first, or together with the first added party, or at the The aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy are interstitially added.
进一步优选地，所述步骤S3可以具体包括：Further preferably, the step S3 may specifically include:
步骤S301，在所述铝熔体中加入所述稀土铝合金并进行熔炼，得到第一均匀混合熔体；Step S301, adding the rare earth aluminum alloy into the aluminum melt and melting to obtain a first homogeneously mixed melt;
步骤S302，在所述第一均匀混合熔体中加入所述铝锶中间合金并继续熔炼，得到第二均匀混合熔体；Step S302, adding the aluminum-strontium master alloy into the first homogeneously mixed melt and continuing to smelt to obtain a second homogeneously mixed melt;
步骤S303，在所述第二均匀混合熔体中加入所述铝钛或铝钛硼中间合金并继续熔炼，得到所述改性铝合金。Step S303, adding the aluminum-titanium or aluminum-titanium-boron master alloy into the second homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
也就是说，通过先加入稀土铝合金并进行熔炼，在此基础上再依次间隔开加入作为变质剂的铝锶中间合金、作为细化剂的铝钛中间合金或铝钛硼中间合金，能够更好地解决锶、硼的毒化作用，得到更细化、更均匀，且机械性能更高的改性铝合金。That is to say, by first adding rare earth aluminum alloy and smelting, and then sequentially adding aluminum-strontium master alloy as a modifier, aluminum-titanium master alloy or aluminum-titanium-boron master alloy as a refiner at intervals on this basis, it can be more refined. The poisoning effect of strontium and boron can be solved well, and a modified aluminum alloy with finer, more uniform and higher mechanical properties can be obtained.
另外，针对改性剂为复合稀土铝合金、铝钛或铝钛硼中间合金的组合，所述步骤S3包括：In addition, for the combination of the modifier being a composite rare earth aluminum alloy, aluminum titanium or aluminum titanium boron master alloy, the step S3 includes:
步骤S310，在所述铝熔体中加入所述复合稀土铝合金并进行熔炼，得到第四均匀混合熔体；Step S310, adding the composite rare earth aluminum alloy into the aluminum melt and melting to obtain a fourth homogeneously mixed melt;
步骤S320，在所述第四均匀混合熔体中加入所述铝钛或铝钛硼中间合金并继续熔炼，得到所述改性铝合金。Step S320, adding the aluminum-titanium or aluminum-titanium-boron master alloy into the fourth homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
也就是说，在事前将稀土铝合金、变质剂、细化剂、铝熔炼制得复合稀土铝合金的情况下，可以一次性加入上述铝熔体中进行制备。当然，考虑到高温熔炼的情况下易于发生晶粒的异常长大，不利于提高其机械性能，优选在复合稀土铝合金全部熔化并与铝合金均匀混合的情况下，在其中进一步加入细化剂即铝钛中间合金或铝钛硼中间合金，控制晶粒生长。That is to say, if the rare earth aluminum alloy, modifier, refining agent, and aluminum are smelted in advance to obtain a composite rare earth aluminum alloy, it can be prepared by adding it to the above aluminum melt at one time. Of course, considering that abnormal growth of crystal grains tends to occur during high-temperature smelting, which is not conducive to improving its mechanical properties, it is preferable to further add a refiner to the composite rare earth aluminum alloy when it is completely melted and mixed with the aluminum alloy. That is, aluminum-titanium master alloy or aluminum-titanium-boron master alloy controls grain growth.
其中，作为改性剂，其添加量根据使用需求、作为中间合金中各有效成分的含量不同而进行相应设计。作为一个示例，例如在通过复合稀土合金(其中所含稀土元素：锶：钛或钛硼总量的质量比＝1：(0.05-1.2)：(0.0001-1))引入的情况下，所述改性剂优选占所述改性铝合金的总量的0.4-0.6wt％。Wherein, as a modifier, its addition amount is designed according to the requirements of use and the content of each active ingredient in the master alloy. As an example, for example, in the case of introducing a composite rare earth alloy (the mass ratio of rare earth elements contained therein: strontium: titanium or the total amount of titanium and boron = 1: (0.05-1.2): (0.0001-1)), the The modifier preferably accounts for 0.4-0.6 wt% of the total amount of the modified aluminum alloy.
进一步地，上述任一步骤中的精炼，即铝熔体纯化过程中的精炼、稀土铝合金制备过程中的精炼、以及复合稀土铝合金中的各熔体的精炼，均可以采用如下方式进行：Further, the refining in any of the above steps, that is, the refining in the process of purifying the aluminum melt, the refining in the process of preparing the rare earth aluminum alloy, and the refining of each melt in the composite rare earth aluminum alloy can be carried out in the following manner:
通过惰性气体吹入精炼剂并保持3-10分钟，此后加入除渣剂并搅拌5-10分钟，并去除表面浮渣。Blow into the refining agent by inert gas and keep it for 3-10 minutes, then add the deslagging agent and stir for 5-10 minutes, and remove the surface scum.
进一步地，所述精炼剂的加入量占所加入的熔体质量的0.1～0.3％，所述 清渣剂的加入量占所加入熔体质量的0.1～0.3％；Further, the addition of the refining agent accounts for 0.1 to 0.3% of the mass of the added melt, and the addition of the slag remover accounts for 0.1 to 0.3% of the mass of the added melt;
所述精炼剂的组分按质量计含有：The components of the refining agent contain by mass:
氯化钾10-15份，氯化钠15-25份，氟化钙8-15份，碳酸钠15-25份，硫酸钠8-12份，氟铝酸钠10-20份，六氯乙烷8-12份；10-15 parts of potassium chloride, 15-25 parts of sodium chloride, 8-15 parts of calcium fluoride, 15-25 parts of sodium carbonate, 8-12 parts of sodium sulfate, 10-20 parts of sodium fluoroaluminate, hexachloroethyl 8-12 parts of alkane;
所述清渣剂的组分按质量计含有：The components of the slag remover contain by mass:
氯化钠25－30份，氯化钾25－30份，碳酸钠5－10份，硫酸钠5－10份，氟铝酸钠1－5份，氟硅酸钠5－10份，氟化钙5－10份，硝酸钾1－5份，氟硅酸钾5－10份。25-30 parts of sodium chloride, 25-30 parts of potassium chloride, 5-10 parts of sodium carbonate, 5-10 parts of sodium sulfate, 1-5 parts of sodium fluoroaluminate, 5-10 parts of sodium fluorosilicate, fluoride 5-10 parts of calcium, 1-5 parts of potassium nitrate, 5-10 parts of potassium fluorosilicate.
进一步地，可以通过监测熔体的氢含量来确定精炼是否继续进行。本发明中，通过测试熔体的密度来估算氢含量，也就是说，熔体密度越接近其理论密度(根据合金中所含成分的不同稍有不同，大致在2.7g/cm 3左右)则表明其中所含氢越低。例如可以设定为，当熔体的密度不足2.65g/cm 3时，则进行所述精炼处理；当熔体密度大于等于2.65g/cm 3，即不进行所述精炼处理或终止所述精炼处理。 Further, it is possible to determine whether refining continues by monitoring the hydrogen content of the melt. In the present invention, the hydrogen content is estimated by testing the density of the melt, that is to say, the closer the melt density is to its theoretical density (slightly different according to the different components contained in the alloy, roughly around 2.7g/cm 3 ), then Indicates that the hydrogen contained in it is lower. For example, it can be set that when the density of the melt is less than 2.65g/cm 3 , the refining process is performed; when the density of the melt is greater than or equal to 2.65g/cm 3 , the refining process is not performed or the refining process is terminated. deal with.
步骤S4，将所述改性铝合金熔体进行浇铸，得到改性铝合金素坯。Step S4, casting the modified aluminum alloy melt to obtain a modified aluminum alloy biscuit.
也就是说，在熔炼之后，将得到的改性铝合金熔体浇铸到模具中，得到所述改性铝合金素坯。That is, after smelting, the obtained modified aluminum alloy melt is cast into a mold to obtain the modified aluminum alloy green body.
具体的浇铸过程，可以采用常规的浇铸工艺，在此省略其详细记载。For the specific casting process, a conventional casting process may be used, and detailed descriptions thereof are omitted here.
步骤S5，对所述改性铝合金素坯进行热处理。Step S5, performing heat treatment on the modified aluminum alloy biscuit.
也就是说，在通过浇铸得到铝合金素坯之后，为了进一步提高其机械强度，发明人在反复研究的基础上，开发出了相应的热处理工艺。That is to say, after the aluminum alloy biscuit is obtained by casting, in order to further improve its mechanical strength, the inventor has developed a corresponding heat treatment process on the basis of repeated research.
具体而言，所述热处理包括：Specifically, the heat treatment includes:
固溶处理，将所述铝合金素坯加热至530-550℃，并保温120-300min；Solution treatment, heating the aluminum alloy biscuit to 530-550°C and keeping it warm for 120-300min;
淬水处理，将经过固溶处理后的铝合金素坯加入温度为60-70℃的水浴中，淬水2-4min；Water quenching treatment, adding the aluminum alloy biscuit after solid solution treatment into a water bath at a temperature of 60-70°C, and quenching water for 2-4 minutes;
时效处理，将经过淬水处理后的铝合金素坯在110-140℃保温120-240min，此后进一步升温至160-200℃并保温20-60min，此后冷却至室温，得到所述高塑性复合改性铝合金制件。For aging treatment, heat the quenched aluminum alloy biscuit at 110-140°C for 120-240 minutes, then further raise the temperature to 160-200°C and hold it for 20-60 minutes, and then cool it to room temperature to obtain the high-plastic composite modification. High-strength aluminum alloy parts.
也就是说，对铝合金素坯先后进行固溶处理、淬水处理、以及时效处理。That is to say, the aluminum alloy biscuit is successively subjected to solution treatment, water quenching treatment, and aging treatment.
通过设计上述固溶处理，能够消除由于铸件结构(如璧厚不均匀、转接处厚大)等原因使铸件在结晶凝固时因冷却速度导致的应力；提高合金的机械强度和硬度，改善金相组织；消除晶间和成分偏析，使组织均匀化。By designing the above solid solution treatment, it is possible to eliminate the stress caused by the cooling rate of the casting due to the structure of the casting (such as uneven wall thickness, thick transition) and other reasons; improve the mechanical strength and hardness of the alloy, and improve the quality of the alloy. Phase structure; eliminate intergranular and component segregation, and make the structure homogeneous.
此外，通过设计上述淬水处理，使铸件急冷，使强化组元在合金中得到最大限度的溶解并固定保存到室温。In addition, by designing the above-mentioned quenching treatment, the casting is rapidly cooled, so that the strengthening components are dissolved in the alloy to the maximum extent and then fixed and stored at room temperature.
进一步地，通过设计上述时效处理，温度的上升和时间的延长，约经过过饱和固溶体点阵内原子的重新组合，生成溶质原子富集区(称为G-PⅠ区)和G-PⅠ区消失，第二相原子按一定规律偏聚并生成G-PⅡ区，生成亚稳定的第二相(过渡相),大量的G-PⅡ区和少量的亚稳定相结合以及亚稳定相转变为稳定相、第二相质点聚集。Further, by designing the above-mentioned aging treatment, the rise of temperature and the extension of time will result in the recombination of atoms in the supersaturated solid solution lattice, forming a solute atom-enriched region (called the G-PI region) and disappearing of the G-PI region. , the atoms of the second phase segregate according to a certain rule and form a G-PII region, forming a metastable second phase (transition phase), a large number of G-PII regions and a small amount of metastable phase combine and the metastable phase transforms into a stable phase , The second phase particle aggregation.
根据本发明的制备方法，首先采用低温时效，使得更多的相变在GP区和β1区，从而能够保证足够的延伸率。According to the preparation method of the present invention, low-temperature aging is first adopted, so that more phase transitions are in the GP region and the β1 region, thereby ensuring sufficient elongation.
优选地，所述固溶处理中的升温速率控制在1.5-3℃/min，保温时间控制在120-180min。通过控制固溶处理的升温速率和保温时间，能够进一步增加蔷薇状α-Al相和较圆整的球形α-Al相，并细化初生α-Al相，减少树枝晶的数量。Preferably, the heating rate in the solution treatment is controlled at 1.5-3°C/min, and the holding time is controlled at 120-180min. By controlling the heating rate and holding time of solution treatment, the rose-like α-Al phase and the rounder spherical α-Al phase can be further increased, the primary α-Al phase can be refined, and the number of dendrites can be reduced.
进一步地，所述固溶处理、所述淬水处理、以及所述时效处理为连续处理，且所述水浴为循环水浴，所述淬水处理后，在进行所述时效处理前所述铸造铝合金素坯的温度保持在55℃以上。通过连续处理，不仅可以提高生产效率，且能够避免工艺中断引入的不必要的缺陷。且控制期间的最低温度，避免由于急速降温引入缺陷。Further, the solid solution treatment, the quenching treatment, and the aging treatment are continuous treatments, and the water bath is a circulating water bath. After the quenching treatment, before the aging treatment, the cast aluminum The temperature of the alloy green body is kept above 55°C. Through continuous processing, not only can production efficiency be increased, but unnecessary defects introduced by process interruption can be avoided. And the lowest temperature during the control period, to avoid the introduction of defects due to rapid cooling.
进一步地，所述时效处理阶段，所述时效处理阶段，从110-140℃以2-4℃/min的升温速率升温至160-200℃，此后自然冷却至室温。通过控制时效处理阶段的降温速率，能够极大地减少缺陷的引入，有助于提高其塑性，且使得机械强度也保持在较高水平。下面，通过具体实施例进一步详细说明根据本发明的制备方法。Further, in the aging treatment stage, in the aging treatment stage, the temperature is raised from 110-140°C to 160-200°C at a heating rate of 2-4°C/min, and then naturally cooled to room temperature. By controlling the cooling rate in the aging treatment stage, the introduction of defects can be greatly reduced, which helps to improve its plasticity and maintain a high level of mechanical strength. Below, the preparation method according to the present invention will be further described in detail through specific examples.
实施例1Example 1
铝合金：采用铝硅镁合金(A356)(购自：山东魏桥铝业)Aluminum alloy: aluminum-silicon-magnesium alloy (A356) (purchased from: Shandong Weiqiao Aluminum Industry)
高纯铝锭(购自中铝集团，成分：Al(99.99％)，Fe<0.1％，杂质<0.05％)High-purity aluminum ingot (purchased from Chinalco, composition: Al (99.99%), Fe<0.1%, impurity<0.05%)
精炼剂：Refining agent:
成分：氯化钾15份，氯化钠20份，CaF2 10份，Na2CO3 20份，Na2SO4 10份，Na3AlF6 15份，C2Cl6 10份。Ingredients: Potassium Chloride 15 parts, Sodium Chloride 20 parts, CaF2 10 parts, Na2CO3 20 parts, Na2SO4 10 parts, Na3AlF6 15 parts, C2Cl6 10 parts.
除渣剂：Deslagging agent:
成分：氯化钠25份，氯化钾25份，碳酸钠5份，硫酸钠5份，氟铝酸钠5份，氟硅酸钠10份，氟化钙10份，硝酸钾5份，氟硅酸钾10份。Ingredients: 25 parts of sodium chloride, 25 parts of potassium chloride, 5 parts of sodium carbonate, 5 parts of sodium sulfate, 5 parts of sodium fluoroaluminate, 10 parts of sodium fluorosilicate, 10 parts of calcium fluoride, 5 parts of potassium nitrate, fluoride Potassium silicate 10 parts.
1)铝合金熔体的制备1) Preparation of aluminum alloy melt
熔化：先将预热的铝硅镁合金A356加到提前升温熔炼炉内，在760度范围内加热熔化成铝水。Melting: first add the preheated aluminum-silicon-magnesium alloy A356 into the pre-heating melting furnace, and heat and melt it into aluminum water within the range of 760 degrees.
除气除渣：熔化成铝水后，通入氮气(或氩气)后吹入精炼剂(0.3wt％精炼剂)到铝水中，通气时间控制在15分钟。Degassing and slag removal: After melting into aluminum water, nitrogen (or argon) is introduced and refining agent (0.3wt% refining agent) is blown into the aluminum water, and the ventilation time is controlled at 15 minutes.
静置：将S3中的铝水静置10分钟，温度控制在760度下，并打捞干净铝水表层的渣杂质。Stand still: let the aluminum water in S3 stand for 10 minutes, the temperature is controlled at 760 degrees, and the slag impurities on the surface of the aluminum water are removed.
期间，对静置的铝水取样测定化学成分并估算氢气量：During this period, the standing aluminum water was sampled to determine the chemical composition and estimate the amount of hydrogen:
以密度法估算其中的氢气含量，密度要求：大于等于2.65g/cm3。当密度越大(越接近2.7g/cm3)则认为其中的氢气含量越低。Estimate the hydrogen content in it by density method, density requirement: greater than or equal to 2.65g/cm3. When the density is greater (closer to 2.7g/cm3), the hydrogen content is considered to be lower.
2)中间合金的纯化处理2) Purification of master alloy
2.1)铝锶中间合金：购自南通昂申金属材料有限公司，成分：Al-10Sr，Fe<0.05。2.1) Al-Sr master alloy: purchased from Nantong Angshen Metal Materials Co., Ltd., composition: Al-10Sr, Fe<0.05.
预处理：用砂轮机将铝锶中间合金的氧化皮和表层处理干净。Pretreatment: Use a grinder to clean the scale and surface of the Al-Sr master alloy.
超声清洗：将预处理后的铝锶中间合金放入超声清洗槽中进行超声处理。Ultrasonic cleaning: put the pretreated aluminum-strontium master alloy into an ultrasonic cleaning tank for ultrasonic treatment.
烘干：将清洗后的铝锶中间合金放入烘箱炉保持60-100℃烘烤30-60分钟。Drying: put the cleaned aluminum-strontium master alloy into an oven and bake at 60-100°C for 30-60 minutes.
熔炼：将铝锶中间合金放入到预热的坩埚中在760-780℃熔化处理。Melting: put the aluminum-strontium master alloy into a preheated crucible and melt it at 760-780°C.
精炼处理：待铝锶中间合金熔化后做精炼处理。通入Ar+石墨自动除气搅拌棒对熔化的高纯铝做精炼处理。在5-10分钟730-750℃时用Ar吹入精炼，吹入精炼剂量在0.1～0.3％熔体，保持在3-5分钟，精炼过程中铝液上表面不能有沸腾气泡。Refining treatment: After the aluminum-strontium master alloy is melted, it is refined. The molten high-purity aluminum is refined by feeding the Ar+graphite automatic degassing stirring rod. Refining with Ar blowing at 730-750°C for 5-10 minutes, the amount of refining being blown in is 0.1-0.3% of the melt, and kept at 3-5 minutes. During the refining process, there should be no boiling bubbles on the upper surface of the aluminum liquid.
表面浮渣清除：在15-20分钟时放入在0.1～0.3％的除渣剂均匀散开，清除表面浮渣。Surface scum removal: Put 0.1-0.3% scum remover in 15-20 minutes and spread evenly to remove surface scum.
静置：扒渣后静置8-15分钟在740-760℃时。Stand still: after removing slag, let stand for 8-15 minutes at 740-760°C.
2.2)细化剂：铝钛硼中间合金的精炼处理2.2) Refining agent: refining treatment of Al-Ti-B master alloy
铝钛硼中间合金：购自南通昂申金属材料有限公司(成分和含量：Ti:5％，B:1％，其余为：Al)Aluminum-titanium-boron master alloy: purchased from Nantong Angshen Metal Materials Co., Ltd. (composition and content: Ti: 5%, B: 1%, the rest: Al)
作为细化剂的铝钛硼中间合金，参考上述进行相同处理。For the aluminum-titanium-boron master alloy used as a refiner, refer to the above and perform the same treatment.
3)复合稀土铝合金的制备3) Preparation of composite rare earth aluminum alloy
3.1)高纯度稀土铝中间合金的熔炼3.1) Melting of high-purity rare earth aluminum master alloy
a)高纯铝熔体的制备a) Preparation of high-purity aluminum melt
预处理：用砂轮机将高纯铝锭表面的氧化皮和表层处理干净。Pretreatment: Use a grinder to clean the oxide skin and surface layer on the surface of the high-purity aluminum ingot.
超声清洗：将预处理后的高纯铝锭放入清洗剂中进行超声处理。Ultrasonic cleaning: Put the pretreated high-purity aluminum ingot into the cleaning agent for ultrasonic treatment.
烘干：将超声清洗后的高纯铝锭中放入烘箱炉保持60-100℃烘烤30-60分钟。Drying: Put the high-purity aluminum ingot after ultrasonic cleaning into an oven and bake at 60-100°C for 30-60 minutes.
熔炼：将烘干后高纯铝放入到预热的坩埚中，在760-800℃加热熔化。Melting: Put the dried high-purity aluminum into a preheated crucible and heat and melt at 760-800°C.
精炼处理：待高纯铝熔化后做精炼处理。具体：通过Ar+石墨自动除气搅拌棒对熔化的高纯铝做精炼处理。在5-10分钟740-760℃时用Ar吹入精炼，吹入精炼剂量在0.1～0.3％熔体，并保持3-5分钟。此后，静置10-20分钟，在其中放入0.1～0.3％的除渣剂使其均匀散开，清除表面浮渣。Refining treatment: Refining treatment is performed after the high-purity aluminum is melted. Specifically: Refining the molten high-purity aluminum through the Ar+graphite automatic degassing stirring rod. Refining by blowing Ar at 740-760°C for 5-10 minutes, the amount of refining being blown in is 0.1-0.3% of the melt, and kept for 3-5 minutes. After that, let it stand for 10-20 minutes, put 0.1-0.3% scum remover in it to make it evenly disperse, and remove the scum on the surface.
静置：扒渣后静置8-15分钟在740-760℃。Stand still: After removing slag, let stand for 8-15 minutes at 740-760°C.
b)稀土铝合金的熔炼：b) Smelting of rare earth aluminum alloys:
将上述a)得到的高纯铝温度调至780-820℃，加热完全熔化后，按设定的质量百分比即在稀土铝合金中镧含量为0.2±0.02wt％加入稀土铝镧合金(购自包头稀土研究院，成分：Al-10La，Fe<0.05)。在氩气气氛保护下在780-820℃下加热使其完全熔化。Adjust the temperature of the high-purity aluminum obtained in the above a) to 780-820° C., and after heating and melting completely, add a rare-earth aluminum-lanthanum alloy (purchased from Baotou Rare Earth Research Institute, composition: Al-10La, Fe<0.05). Under the protection of argon atmosphere, heat it at 780-820°C to make it melt completely.
搅拌和保温：对熔化后的熔体搅拌3-5分钟使其均匀化，在760-780℃时对熔体保温10-20分钟。Stirring and heat preservation: Stir the melted melt for 3-5 minutes to make it homogeneous, and keep the melt at 760-780°C for 10-20 minutes.
精炼处理：整体过程在氩气气氛保护下，待稀土铝镧合金熔化后做精炼处理。通入Ar+石墨自动除气搅拌棒对熔化的其做精炼处理。在5-10分钟760-780℃时用Ar吹入精炼，吹入精炼剂量在0.1～0.3％熔体，保持在3-5分钟，精炼过程中铝液上表面不能有沸腾气泡。对熔体表面浮渣清除：在15-20分钟时放入 在0.1～0.3％的除渣剂均匀散开，清除表面浮渣。Refining treatment: The whole process is under the protection of argon atmosphere, and the refining treatment is performed after the rare earth aluminum-lanthanum alloy is melted. Feed the Ar+graphite automatic degassing stirring rod to refine the melted one. Refining with Ar blowing at 760-780°C for 5-10 minutes, the amount of refining being blown in is 0.1-0.3% of the melt, and kept at 3-5 minutes. During the refining process, there should be no boiling bubbles on the upper surface of the aluminum liquid. Remove scum on the surface of the melt: put in 0.1-0.3% slag remover in 15-20 minutes and spread evenly to remove the scum on the surface.
静置：扒渣后在720-730℃静置10-15分钟。Stand still: after removing slag, let stand at 720-730°C for 10-15 minutes.
3.2)复合稀土合金的制备3.2) Preparation of composite rare earth alloy
经过上述分别准备了铝熔体、稀土铝合金、铝锶中间合金、以及铝钛硼中间合金，接下来，对其进行混合熔炼，以得到复合稀土合金。The aluminum melt, the rare earth aluminum alloy, the aluminum-strontium master alloy, and the aluminum-titanium-boron master alloy are respectively prepared through the above, and then mixed and smelted to obtain a composite rare earth alloy.
本实施中，作为添加顺序，首先在铝熔体中添加稀土铝合金，接着添加铝锶合金，最终添加铝钛硼合金。具体如下：In this embodiment, as an addition sequence, the rare earth aluminum alloy is firstly added to the aluminum melt, then the aluminum strontium alloy is added, and finally the aluminum titanium boron alloy is added. details as follows:
步骤1、配料：将上述得到的高纯铝、铝钛硼中间合金、铝锶中间合金、稀土铝合金按要求的质量百分比称量后预热。Step 1. Ingredients: Preheat the high-purity aluminum, aluminum-titanium-boron master alloy, aluminum-strontium master alloy, and rare earth aluminum alloy obtained above according to the required mass percentage.
以总重量100份计，高纯铝：4.8份、铝钛硼中间合金：0.2份、铝锶中间合金：60份、稀土铝合金：35份。Based on 100 parts by total weight, high-purity aluminum: 4.8 parts, aluminum-titanium-boron master alloy: 0.2 parts, aluminum-strontium master alloy: 60 parts, and rare earth aluminum alloy: 35 parts.
步骤2、加入并熔化稀土铝合金：对于上述铝熔体，首先将上述经纯化处理的稀土铝合金加热至780～820℃使其在熔化前软化，此后将铝熔体整体温度控制在760～780℃，将稀土铝合金加入铝熔体中进行保温。Step 2. Adding and melting the rare earth aluminum alloy: For the above aluminum melt, first heat the above purified rare earth aluminum alloy to 780-820°C to soften before melting, and then control the overall temperature of the aluminum melt at 760-820°C 780°C, add rare earth aluminum alloy into the aluminum melt for heat preservation.
整体过程采用氩气氛围保护，熔化稀土铝合金。The whole process adopts the protection of argon atmosphere and melts the rare earth aluminum alloy.
步骤3、待稀土铝合金完全熔化后，将温度控制在750～770℃时，进行搅拌5-10分钟。Step 3. After the rare earth aluminum alloy is completely melted, the temperature is controlled at 750-770° C. and stirred for 5-10 minutes.
整体过程采用氩气氛围保护，搅拌棒采用石墨材料并使其在搅拌前预热到400-500℃。The whole process is protected by an argon atmosphere, and the stirring rod is made of graphite material and preheated to 400-500°C before stirring.
也就是说，在稀土铝合金完全熔化后，稍稍降低温度，可以防止过热引起后续晶粒粗化等。That is to say, after the rare earth aluminum alloy is completely melted, lowering the temperature slightly can prevent subsequent grain coarsening caused by overheating.
步骤4、对熔化后的熔体在740～760℃下，保温时间控制在5-20分钟进行保温处理。该阶段中，发生合金化反应。Step 4, heat-preserve the melted melt at 740-760° C. and control the heat-retaining time within 5-20 minutes. In this stage, an alloying reaction occurs.
步骤5、精炼：保温结束后，进行精炼、除气除渣。在熔体中通过氩气吹入0.3％的精炼剂，通气时间控制在3～8分钟；此后，进一步加入0.2％的除渣剂中，搅拌5分钟静置并去除熔体表层的渣及杂质。整体过程采用氩气氛围保护。Step 5. Refining: After the heat preservation is completed, refining, degassing and slag removal are carried out. 0.3% refining agent is blown into the melt by argon, and the aeration time is controlled at 3 to 8 minutes; after that, further add 0.2% slag remover, stir for 5 minutes and let stand to remove the slag and impurities on the surface of the melt . The whole process is protected by argon atmosphere.
在精炼前以及精炼过程中铝熔体取样，测定其密度以估算氢含量。测量方法采用密度法(以铝的理论值2.70g/cm3做对比)，测量的样品越是接近2.7g/cm3， 表示铝的内部氢含量越低。一般正常达不到2.7g/cm3；样品的密度测试大约等于2.65g/cm3即可估算氢含量过程中必须抽真空处理，若氢含量不合格，则进一步进行精炼，即重复加入精炼剂、除渣剂再一次精炼。The aluminum melt is sampled before and during refining and its density is determined to estimate the hydrogen content. The measurement method adopts the density method (compared with the theoretical value of aluminum of 2.70g/cm3), the closer the measured sample is to 2.7g/cm3, the lower the internal hydrogen content of aluminum. Generally, it cannot reach 2.7g/cm3 normally; the density test of the sample is about 2.65g/cm3 to estimate the hydrogen content. During the process, the hydrogen content must be vacuumized. The slag agent is refined again.
步骤6、静置：将加入稀土铝合金并精炼后的熔体静置3-5分钟，温度控制在740-760度下。Step 6. Stand still: put the melt that has been added with the rare earth aluminum alloy and refined for 3-5 minutes, and the temperature is controlled at 740-760 degrees.
步骤7、加入并熔化铝锶中间合金：将上述精炼后的铝锶中间合金加入步骤6的熔体中，将温度控制在780～820℃，使得铝锶中间合金完全熔化。整体过程采用氩气氛围保护，熔化铝锶中间合金。Step 7. Adding and melting the aluminum-strontium master alloy: adding the above-mentioned refined aluminum-strontium master alloy into the melt in step 6, and controlling the temperature at 780-820° C. to completely melt the aluminum-strontium master alloy. The whole process is protected by argon atmosphere, and the aluminum-strontium master alloy is melted.
步骤8、待铝锶中间合金熔化后，将温度控制在740～760℃，搅拌3-8分钟，实现均质化。整体过程采用氩气氛围保护，搅拌棒采用石墨材料，搅拌前预热到400-500℃。Step 8. After the aluminum-strontium master alloy is melted, control the temperature at 740-760° C. and stir for 3-8 minutes to achieve homogenization. The whole process is protected by argon atmosphere, the stirring rod is made of graphite material, and it is preheated to 400-500°C before stirring.
步骤9、接下来，在725～750℃下，进行保温处理。保温时间控制在15-30分钟。Step 9. Next, heat preservation treatment is carried out at 725-750°C. The heat preservation time is controlled at 15-30 minutes.
步骤10、精炼、除气除渣：待熔体保温结束后，通入氩气后吹入精炼剂0.3％到铝稀土复合熔体中，通气时间控制在5～10分钟；放入0.2％的扒渣剂到铝熔体中，搅拌5分钟并打捞铝稀土复合熔体表层的渣及杂质。整体过程采用氩气氛围保护。Step 10. Refining, degassing and slag removal: After the heat preservation of the melt is completed, blow in 0.3% of the refining agent into the aluminum-rare-earth composite melt after argon gas is introduced, and the ventilation time is controlled at 5 to 10 minutes; put in 0.2% of Put the slag removal agent into the aluminum melt, stir for 5 minutes and remove the slag and impurities on the surface of the aluminum-rare-earth composite melt. The whole process is protected by argon atmosphere.
在精炼前以及精炼过程中铝熔体取样，测定氢含量。(氢气含量要求：大于等于2.65g/cm 3；)测氢过程中必须抽真空处理，若氢含量不合格，则进一步进行精炼，即重复加入精炼剂、除渣剂再一次精炼。 The aluminum melt is sampled before and during refining to determine the hydrogen content. (Hydrogen content requirement: greater than or equal to 2.65g/cm 3 ;) During the hydrogen measurement process, it must be vacuumized. If the hydrogen content is unqualified, then further refining, that is, adding refining agents and slag removers to refine again.
步骤11、加铝钛硼中间合金：在上述步骤10处理后的熔体中，加入铝钛硼中间合金，加热使其完全熔化，并均匀搅拌3-5分钟使其均质化。Step 11. Add Al-Ti-B master alloy: Add Al-Ti-B master alloy to the melt treated in Step 10 above, heat to melt completely, and stir evenly for 3-5 minutes to homogenize.
步骤12、保温：搅拌后，将熔体保温8-12分钟，温度控制在715-725℃下。Step 12, heat preservation: after stirring, heat the melt for 8-12 minutes, and control the temperature at 715-725°C.
步骤13、精炼、除气除渣：待熔体保温结束后，通入氩气后吹入精炼剂0.3％到铝稀土复合熔体中，通气时间控制在5～10分钟；放入0.2％的扒渣剂到铝熔体中，搅拌5分钟并打捞铝稀土复合熔体表层的渣及杂质。整体过程采用氩气氛围保护。Step 13. Refining, degassing and slag removal: After the heat preservation of the melt is completed, blow in 0.3% of the refining agent into the aluminum-rare-earth composite melt after argon gas is introduced, and the ventilation time is controlled at 5 to 10 minutes; put in 0.2% of Put the slag removal agent into the aluminum melt, stir for 5 minutes and remove the slag and impurities on the surface of the aluminum-rare-earth composite melt. The whole process is protected by argon atmosphere.
在精炼前以及精炼过程中铝熔体取样，测定氢含量。(氢气含量要求：大 于等于2.65g/cm 3；)测氢过程中必须抽真空处理，若氢含量不合格，则进一步进行精炼，即重复加入精炼剂、除渣剂再一次精炼，直至合格。 The aluminum melt is sampled before and during refining to determine the hydrogen content. (Hydrogen content requirement: greater than or equal to 2.65g/cm 3 ;) Vacuum treatment must be performed during the hydrogen measurement process. If the hydrogen content is unqualified, further refining is carried out, that is, refining agents and slag removers are added repeatedly until it is qualified.
步骤14、浇铸：模具预热在300-400℃。将上述步骤13得到的复合稀土合金熔体温度控制在715～725℃浇铸即可。Step 14, casting: the mold is preheated at 300-400°C. The temperature of the composite rare earth alloy melt obtained in step 13 above is controlled at 715-725° C. for casting.
优选地，浇铸时，铝稀土复合熔体表层的氧化物采用玻璃纤维的过滤网过滤干净；每次浇铸前对铝稀土复合熔体表层做过滤处理后浇铸。Preferably, during casting, the oxides on the surface of the aluminum-rare-earth composite melt are filtered through a glass fiber filter; before each casting, the surface of the aluminum-rare-earth composite melt is filtered before casting.
优选地，浇铸的模具冷却控制，对浇铸到模具中铝稀土复合熔体采用水冷方式冷却，冷却过程中，采用以50-100℃/s控制铝熔体凝固速度，凝固方式用顺序凝固。Preferably, the cooling control of the casting mold adopts a water cooling method to cool the aluminum-rare-earth composite melt cast into the mold. During the cooling process, the solidification speed of the aluminum melt is controlled at 50-100°C/s, and the solidification method is sequential solidification.
需要说明的是，复合稀土铝合金的成分比例并不受上述实施例的限制，例如，可以设计为所述稀土金属：锶：钛或钛硼重量的质量比为1:(0.1-1.2)：(0.1-1.2)。It should be noted that the composition ratio of the composite rare earth aluminum alloy is not limited by the above embodiments, for example, it can be designed such that the mass ratio of the rare earth metal: strontium: titanium or titanium boron weight is 1: (0.1-1.2): (0.1-1.2).
4)改性铝合金素坯的制备4) Preparation of modified aluminum alloy bisque
以铝合金：复合稀土铝合金：铝钛硼中间合金的质量比为99.4：0.4：0.2的比例准备上述铝硅镁合金、复合稀土铝合金、以及铝钛硼中间合金。The aluminum-silicon-magnesium alloy, the composite rare-earth aluminum alloy, and the aluminum-titanium-boron master alloy are prepared with a mass ratio of aluminum alloy:composite rare earth aluminum alloy:aluminium-titanium-boron master alloy of 99.4:0.4:0.2.
此后，按照如下步骤进行熔炼。Thereafter, smelting is carried out as follows.
混合：按照上述比例，在上述1)处理后的铝硅镁合金熔体中，将温度控制在740±5度时，首先加入3)得到的复合稀土铝合金。Mixing: According to the above ratio, in the above 1) treated aluminum-silicon-magnesium alloy melt, when the temperature is controlled at 740±5 degrees, first add the composite rare earth aluminum alloy obtained in 3) first.
搅拌：用石墨搅拌器对加入复合稀土铝合金并熔化的熔体进行搅拌，搅拌过程中需要均匀搅拌，连续搅拌8分钟；Stirring: use graphite stirrer to stir the melt which is added with composite rare earth aluminum alloy and melted. During the stirring process, uniform stirring is required and continuous stirring is required for 8 minutes;
保温：搅拌后将温度控制在735度进行保温，保温时间控制在20分钟；Heat preservation: After stirring, control the temperature at 735 degrees for heat preservation, and the heat preservation time is controlled at 20 minutes;
精炼：保温结束后，通入氩气后用吹入清渣剂到铝水中，通气时间控制在15分钟；Refining: After the heat preservation is over, blow into the aluminum water with argon gas and blow the slag cleaning agent into the aluminum water, and the ventilation time is controlled at 15 minutes;
加入细化剂：加入0.2％铝钛硼中间合金到精炼的铝水中，待其熔化搅拌并持续进行精炼；Add refiner: add 0.2% Al-Ti-B intermediate alloy to the refined aluminum water, wait for it to melt and stir and continue refining;
保温静置：精炼结束后，铝水流入保温池后，温度控制在710±3度时，静置10±2分钟后去除铝水表层的渣、杂质；Heat preservation and standing: After refining, the aluminum water flows into the heat preservation pool, and when the temperature is controlled at 710±3 degrees, the slag and impurities on the surface of the aluminum water are removed after standing for 10±2 minutes;
浇铸：预热模具在250-400度时，将上述温度控制在700±5的精炼后改性铝合金浇铸到模具中，冷却即得到改性铝合金素坯。其中，该改性铝合金素坯 的厚度为30mm。Casting: When the mold is preheated at 250-400 degrees, the refined modified aluminum alloy with the above temperature controlled at 700±5 is cast into the mold, and the modified aluminum alloy biscuit is obtained after cooling. Wherein, the thickness of the modified aluminum alloy biscuit is 30mm.
5)热处理5) heat treatment
固溶处理：将上述改性铝合金素坯至于加热炉中，以2℃/min的加热速率加热至540℃，并在此保温120min。Solution treatment: put the modified aluminum alloy biscuit in a heating furnace, heat it to 540°C at a heating rate of 2°C/min, and keep it there for 120min.
淬水处理，将上述固溶处理后的改性铝合金素坯加入温度为65℃的循环水浴中，淬水3min。For water quenching treatment, the modified aluminum alloy biscuit after the above solid solution treatment is added into a circulating water bath at a temperature of 65° C., and water is quenched for 3 minutes.
时效处理，将经过淬水处理后的改性铝合金素坯直接放入120℃的保温箱保温120min，此后以2℃/min的升温速率升温至160℃并保温30min，此后自然冷却至室温，得到所述高塑性复合改性铝合金制件。For aging treatment, put the modified aluminum alloy biscuit after water quenching directly into an incubator at 120°C for 120 minutes, then raise the temperature to 160°C at a heating rate of 2°C/min and hold it for 30 minutes, then cool naturally to room temperature. The high-plastic composite modified aluminum alloy product is obtained.
图1示出了不同阶段铝合金制件的金相组织图像，其中，(a)为热处理前的A356铝合金的图像，(b)为热处理后的A356铝合金的图像，(c)为实施例1中复合改性后、热处理前的图像，(d)为实施例1的复合改性并进行热处理后的图像。由图1可知，本实施例的改性、热处理后的铝合金的金相组织，较圆整的球形α-Al相进一步增加，初生α-Al相以及树枝晶基本不可见。也就是说，晶粒进一步均质化，微观结构更加均匀。另外，球形α-Al相均匀分布在晶界处。且热处理后的铝合金的金相组织(即(c))，较圆整的球形α-Al相进一步增加，初生α-Al相以及树枝晶基本不可见。也就是说，晶粒进一步均质化，微观结构更加均匀。Fig. 1 shows the metallographic structure images of aluminum alloy parts in different stages, wherein, (a) is the image of A356 aluminum alloy before heat treatment, (b) is the image of A356 aluminum alloy after heat treatment, (c) is the The image after compound modification and before heat treatment in Example 1, (d) is the image after compound modification and heat treatment in Example 1. It can be seen from Figure 1 that the metallographic structure of the modified and heat-treated aluminum alloy in this embodiment is further increased compared with the rounded spherical α-Al phase, and the primary α-Al phase and dendrites are basically invisible. That is to say, the grains are further homogenized and the microstructure is more uniform. In addition, the spherical α-Al phase is uniformly distributed at the grain boundaries. Moreover, the metallographic structure of the aluminum alloy after heat treatment (ie (c)) is further increased compared with the round spherical α-Al phase, and the primary α-Al phase and dendrites are basically invisible. That is to say, the grains are further homogenized and the microstructure is more uniform.
另外，对A356铝合金(记作：改性前)、改性后素坯(记作：改性合金1)、以及热处理后的制件(记作：实施例1)的机械性能进行了评价。评价结果示于下述表1。In addition, the mechanical properties of the A356 aluminum alloy (denoted as: before modification), the green body after modification (denoted as: modified alloy 1), and the product after heat treatment (denoted as: Example 1) were evaluated. . The evaluation results are shown in Table 1 below.
表1实施例1的高强度复合改性铝合金制件的机械性能评价结果Table 1 The mechanical performance evaluation results of the high-strength composite modified aluminum alloy parts of Example 1
机械性能Mechanical behavior 改性前Before modification 改性合金1Modified Alloy 1 实施例1Example 1
抗拉强度(MPa)Tensile strength (MPa) 130±3.5130±3.5 220±5220±5 280±6280±6
屈服强度(MPa)Yield strength (MPa) 65±5.565±5.5 108±6108±6 200±5200±5
延伸率(％)Elongation (%) 3±0.253±0.25 20±0.620±0.6 16±0.516±0.5
由表1可知，通过本实施例1的热处理，即便未进行热处理，也能够很大 地提高其塑性。在结合热处理的基础上，极大地提高了其屈服强度、以及抗拉强度(相对于未改性、未进行热处理的铝合金母锭而言，屈服轻度以及抗拉强度分别增加了近3倍、超2倍)，同时也保持了较高水平的延伸率(相对于未处理的铝合金母锭而言，提高了超5倍)，极大地提高了综合机械性能。As can be seen from Table 1, through the heat treatment in Example 1, even without heat treatment, the plasticity can be greatly improved. On the basis of combined heat treatment, its yield strength and tensile strength are greatly improved (compared to the unmodified and unheated aluminum alloy master ingot, the yield strength and tensile strength are increased by nearly 3 times respectively , more than 2 times), while maintaining a high level of elongation (compared to the untreated aluminum alloy master ingot, it has increased by more than 5 times), which greatly improves the comprehensive mechanical properties.
实施例2Example 2
本实施例中，与上述实施例1相比，除了改性剂使用稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金的组合，其余与实施例1相同。In this embodiment, compared with the above-mentioned embodiment 1, except that the modifier uses a combination of rare earth aluminum alloy, aluminum-strontium master alloy, aluminum-titanium or aluminum-titanium-boron master alloy, the rest is the same as embodiment 1.
下面，仅针对改性铝合金熔体的处理中涉及不同的部分进行描述如下：Below, only the different parts involved in the treatment of the modified aluminum alloy melt are described as follows:
4)改性铝合金素坯的制备4) Preparation of modified aluminum alloy bisque
以铝合金：稀土铝合金(稀土铝合金的纯化处理同实施例1)：铝锶合金：铝钛硼中间合金的质量比为99.4：0.2：0.2：0.2的比例准备上述铝硅镁合金、稀土铝合金、铝锶中间合金、以及铝钛硼中间合金。With aluminum alloy: rare earth aluminum alloy (the purification treatment of rare earth aluminum alloy is the same as in Example 1): aluminum strontium alloy: aluminum titanium boron intermediate alloy mass ratio is the ratio of 99.4:0.2:0.2:0.2 to prepare the above-mentioned aluminum silicon magnesium alloy, rare earth Aluminum alloys, aluminum-strontium master alloys, and aluminum-titanium-boron master alloys.
此后，按照如下步骤进行熔炼。Thereafter, smelting is carried out as follows.
混合：按照上述比例，在上述1)处理后的铝硅镁合金熔体中，将温度控制在740±5度时，首先加入稀土铝合金。Mixing: According to the above ratio, in the aluminum-silicon-magnesium alloy melt after the treatment in the above 1), when the temperature is controlled at 740±5 degrees, the rare earth aluminum alloy is firstly added.
搅拌：用石墨搅拌器对加入稀土铝合金并熔化的熔体进行搅拌，搅拌过程中需要均匀搅拌，连续搅拌8分钟；Stirring: use graphite stirrer to stir the melted melt with rare earth aluminum alloy added, uniform stirring is required during the stirring process, continuous stirring for 8 minutes;
保温：搅拌后将温度控制在735度进行保温，保温时间控制在20分钟；Heat preservation: After stirring, control the temperature at 735 degrees for heat preservation, and the heat preservation time is controlled at 20 minutes;
精炼：保温结束后，通入氩气后用吹入清渣剂到铝水中，通气时间控制在15分钟；Refining: After the heat preservation is over, blow into the aluminum water with argon gas and blow the slag cleaning agent into the aluminum water, and the ventilation time is controlled at 15 minutes;
加入铝锶中间合金：加入0.2％铝锶中间合金到精炼的铝水中，待其熔化搅拌并持续进行精炼；Add aluminum-strontium master alloy: add 0.2% aluminum-strontium master alloy to the refined aluminum water, wait for it to melt and stir and continue refining;
均质化：待铝锶中间合金完全熔化后，将温度控制在740～760℃，搅拌3-8分钟，实现均质化；Homogenization: After the Al-Sr master alloy is completely melted, control the temperature at 740-760°C and stir for 3-8 minutes to achieve homogenization;
保温：接下来，在725～750℃下，进行保温处理，保温时间控制在15-30分钟；Heat preservation: Next, heat preservation treatment is carried out at 725-750°C, and the heat preservation time is controlled at 15-30 minutes;
加入细化剂：加入0.2％铝钛硼中间合金到精炼的铝水中，待其熔化搅拌并持续进行精炼；Add refiner: add 0.2% Al-Ti-B intermediate alloy to the refined aluminum water, wait for it to melt and stir and continue refining;
保温静置：精炼结束后，铝水流入保温池后，温度控制在710±3度时，静置10±2分钟后去除铝水表层的渣、杂质；Heat preservation and standing: After refining, the aluminum water flows into the heat preservation pool, and when the temperature is controlled at 710±3 degrees, the slag and impurities on the surface of the aluminum water are removed after standing for 10±2 minutes;
浇铸：预热模具在250-400度时，将上述温度控制在700±5的精炼后改性铝合金浇铸到模具中，冷却即得到改性铝合金素坯。Casting: When the mold is preheated at 250-400 degrees, the refined modified aluminum alloy with the above temperature controlled at 700±5 is cast into the mold, and the modified aluminum alloy biscuit is obtained after cooling.
本实施例得到的产品的金相组织图像和实施例1相似，在此不再详细说明。The metallographic structure image of the product obtained in this embodiment is similar to that of embodiment 1, and will not be described in detail here.
表2实施例2的高强度复合改性铝合金制件的机械性能评价结果Table 2 The mechanical performance evaluation results of the high-strength composite modified aluminum alloy parts of Example 2
机械性能Mechanical behavior 改性前Before modification 改性合金2Modified Alloy 2 实施例2Example 2
抗拉强度(MPa)Tensile strength (MPa) 130±3.5130±3.5 200±5.5200±5.5 240±3.5240±3.5
屈服强度(MPa)Yield strength (MPa) 65±5.565±5.5 95±4.295±4.2 180±3.8180±3.8
延伸率(％)Elongation (%) 3±0.253±0.25 16.6±0.3516.6±0.35 14.2±0.3514.2±0.35
其中，改性合金2表示改性后素坯，未进行热处理。Among them, the modified alloy 2 represents the green body after modification without heat treatment.
由表2可知，通过本实施例2的热处理，也能够得到与上述实施例1相类似的结果。It can be seen from Table 2 that the heat treatment in this embodiment 2 can also obtain similar results to the above-mentioned embodiment 1.
同时可知，相比于实施例2而言，首先将稀土铝合金和铝锶中间合金进行熔炼以制备复合稀土铝合金，并利用该复合稀土铝合金进行改性所得到的复合改性铝合金制件(即实施例1)具有更高的综合机械性能。At the same time, it can be seen that, compared with Example 2, the rare earth aluminum alloy and the aluminum strontium master alloy are first smelted to prepare a composite rare earth aluminum alloy, and the composite modified aluminum alloy obtained by modifying the composite rare earth aluminum alloy is Part (i.e. embodiment 1) has higher comprehensive mechanical properties.
实施例3Example 3
本实施例中，与上述实施例1相比，除了代替使用A356而使用ZL111外，其余均相同。In this embodiment, compared with the above-mentioned embodiment 1, except that ZL111 is used instead of A356, the rest are the same.
具体的制备参考实施例1，在此省略其详细说明。For specific preparation, refer to Example 1, and its detailed description is omitted here.
另外，对ZL111铝合金(记作：改性前)、改性后素坯(记作：改性合金3)、以及热处理后的制件(记作：实施例3)的机械性能进行了评价。评价结果示于下述表3。In addition, the mechanical properties of the ZL111 aluminum alloy (denoted as: before modification), the green body after modification (denoted as: modified alloy 3), and the product after heat treatment (denoted as: Example 3) were evaluated. . The evaluation results are shown in Table 3 below.
表3实施例3的高强度复合改性铝合金制件的机械性能评价结果Table 3 The mechanical performance evaluation results of the high-strength composite modified aluminum alloy parts of Example 3
机械性能Mechanical behavior 改性前Before modification 改性合金3Modified Alloy 3 实施例3Example 3
抗拉强度(MPa)Tensile strength (MPa) 160±4.5160±4.5 240±5240±5 330±6330±6
屈服强度(MPa)Yield strength (MPa) 75±4.575±4.5 120±5120±5 220±4.5220±4.5
延伸率(％)Elongation (%) 3±0.253±0.25 15±0.515±0.5 12±0.512±0.5
由表3可知，通过本实施例3的热处理，也能够得到与上述实施例1、2相类似的结果。也就是说，本发明的制备工艺同样适用于共晶型铝合金，能够获得更好的强度与更高的韧性。It can be seen from Table 3 that the heat treatment in Example 3 can also obtain similar results to those in Examples 1 and 2 above. That is to say, the preparation process of the present invention is also applicable to the eutectic aluminum alloy, which can obtain better strength and higher toughness.
以上所述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，在不脱离本发明所述原理的前提下，还可以作出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。The above description is 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 (11)

  1. 一种高塑性复合改性铝合金制件的制备方法，其特征在于，包括如下步骤：A method for preparing a high-plastic composite modified aluminum alloy product, characterized in that it comprises the following steps:
    步骤S1，提供铝合金熔体；Step S1, providing an aluminum alloy melt;
    步骤S2，提供改性剂；Step S2, providing a modifier;
    其中，所述改性剂为稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金的组合，Wherein, the modifier is a combination of rare earth aluminum alloy, aluminum-strontium master alloy, aluminum-titanium or aluminum-titanium-boron master alloy,
    或者所述改性剂为复合稀土铝合金、铝钛或铝钛硼中间合金的组合，所述复合稀土铝合金中含有锶、钛或钛硼、以及稀土金属，Or the modifier is a combination of composite rare earth aluminum alloy, aluminum titanium or aluminum titanium boron intermediate alloy, and the composite rare earth aluminum alloy contains strontium, titanium or titanium boron, and rare earth metals,
    所述稀土铝合金、所述复合稀土铝合金中的稀土金属为镧、铈、钇中的任意一种或多种；The rare earth metal in the rare earth aluminum alloy and the composite rare earth aluminum alloy is any one or more of lanthanum, cerium, and yttrium;
    步骤S3，在惰性气体气氛下，在所述铝合金熔体中，加入所述改性剂并熔炼，得到改性铝合金熔体；Step S3, adding the modifying agent to the aluminum alloy melt under an inert gas atmosphere and melting to obtain a modified aluminum alloy melt;
    步骤S4，利用所述改性铝合金熔体进行浇铸，得到改性铝合金素坯；Step S4, using the modified aluminum alloy melt to perform casting to obtain a modified aluminum alloy biscuit;
    步骤S5，对所述改性铝合金素坯进行热处理，其中，所述热处理包括：Step S5, performing heat treatment on the modified aluminum alloy green body, wherein the heat treatment includes:
    固溶处理，将所述改性铝合金素坯加热至530-550℃，并保温120-300min；Solution treatment, heating the modified aluminum alloy biscuit to 530-550°C, and keeping it warm for 120-300min;
    淬水处理，将经过固溶处理后的改性铝合金素坯加入温度为60-70℃的水浴中，淬水2-4min；Water quenching treatment, adding the modified aluminum alloy biscuit after solid solution treatment into a water bath at a temperature of 60-70°C, and quenching water for 2-4 minutes;
    时效处理，将经过淬水处理后的铝合金素坯在110-140℃保温120-240min，此后进一步升温至160-200℃并保温20-60min，此后冷却至室温，得到所述高塑性复合改性铝合金制件。For aging treatment, heat the quenched aluminum alloy biscuit at 110-140°C for 120-240min, then further raise the temperature to 160-200°C and hold it for 20-60min, and then cool it to room temperature to obtain the high-plastic composite modification. High-strength aluminum alloy parts.
  2. 根据权利要求1所述的制备方法，其特征在于，所述步骤S1包括：The preparation method according to claim 1, wherein said step S1 comprises:
    提供铝合金母锭；Provide aluminum alloy master ingot;
    去除所述铝合金母锭的表面氧化皮层并进行清洗、烘干；removing the oxide skin layer on the surface of the aluminum alloy master ingot, cleaning and drying;
    将烘干后的铝合金母锭进行熔炼，并进行精炼、除渣，得到所述铝合金熔体，Melting the dried aluminum alloy mother ingot, refining and removing slag to obtain the aluminum alloy melt,
    其中，所述铝合金母锭的成分为亚共晶铝合金或共晶铝合金。Wherein, the composition of the aluminum alloy master ingot is hypoeutectic aluminum alloy or eutectic aluminum alloy.
  3. 根据权利要求1所述的制备方法，其特征在于，所述改性剂为稀土铝 合金、铝锶中间合金、铝钛或铝钛硼中间合金的组合，其中，所述铝锶中间合金与所述铝钛或铝钛硼中间合金间隔开加入，The preparation method according to claim 1, wherein the modifier is a combination of rare earth aluminum alloy, aluminum-strontium master alloy, aluminum-titanium or aluminum-titanium-boron master alloy, wherein the aluminum-strontium master alloy and the The aluminum-titanium or aluminum-titanium-boron master alloy is added at intervals,
    所述稀土铝合金最先加入，或者与首先加入的一方一同加入，或者在所述铝锶中间合金与所述铝钛或铝钛硼中间合金加入间隙加入。The rare earth aluminum alloy is added first, or added together with the first added party, or added between the addition of the aluminum-strontium master alloy and the aluminum-titanium or aluminum-titanium-boron master alloy.
  4. 根据权利要求3所述的制备方法，其特征在于，所述步骤S3包括：The preparation method according to claim 3, wherein said step S3 comprises:
    步骤S301，在所述铝合金熔体中加入所述稀土铝合金并进行熔炼，得到第一均匀混合熔体；Step S301, adding the rare earth aluminum alloy into the aluminum alloy melt and melting to obtain a first homogeneously mixed melt;
    步骤S302，在所述第一均匀混合熔体中加入所述铝锶中间合金并继续熔炼，得到第二均匀混合熔体；Step S302, adding the aluminum-strontium master alloy into the first homogeneously mixed melt and continuing to smelt to obtain a second homogeneously mixed melt;
    步骤S303，在所述第二均匀混合熔体中加入所述铝钛或铝钛硼中间合金并继续熔炼，得到所述改性铝合金。Step S303, adding the aluminum-titanium or aluminum-titanium-boron master alloy into the second homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
  5. 根据权利要求1所述的制备方法，其特征在于，所述改性剂为复合稀土铝合金、铝钛或铝钛硼中间合金的组合，所述步骤S3包括：The preparation method according to claim 1, wherein the modifying agent is a combination of composite rare earth aluminum alloy, aluminum titanium or aluminum titanium boron intermediate alloy, and the step S3 includes:
    步骤S310，在所述铝合金熔体中加入所述复合稀土铝合金并进行熔炼，得到第四均匀混合熔体；Step S310, adding the composite rare earth aluminum alloy into the aluminum alloy melt and melting to obtain a fourth uniformly mixed melt;
    步骤S320，在所述第四均匀混合熔体中加入所述铝钛或铝钛硼中间合金并继续熔炼，得到所述改性铝合金。Step S320, adding the aluminum-titanium or aluminum-titanium-boron master alloy into the fourth homogeneously mixed melt and continuing melting to obtain the modified aluminum alloy.
  6. 根据权利要求5所述的制备方法，其特征在于，所述复合稀土铝合金的制备包括：The preparation method according to claim 5, wherein the preparation of the composite rare earth aluminum alloy comprises:
    步骤S211，提供所述铝熔体；Step S211, providing the aluminum melt;
    步骤S212，提供铝锶中间合金、铝钛或铝钛硼中间合金、以及稀土铝中间合金，所述稀土铝中间合金中的稀土金属为选自镧、铈、钇中的一种或多种；Step S212, providing an aluminum-strontium master alloy, an aluminum-titanium or aluminum-titanium-boron master alloy, and a rare earth aluminum master alloy, wherein the rare earth metal in the rare earth aluminum master alloy is one or more selected from lanthanum, cerium, and yttrium;
    步骤S213，在惰性气体气氛下，在所述铝熔体中，依次加入所述稀土铝合金、铝锶中间合金、铝钛或铝钛硼中间合金并熔炼，得到所述复合稀土合金。Step S213 , under an inert gas atmosphere, sequentially add the rare earth aluminum alloy, aluminum strontium master alloy, aluminum titanium or aluminum titanium boron master alloy into the aluminum melt and melt to obtain the composite rare earth alloy.
  7. 根据权利要求1所述的制备方法，其特征在于，所述改性剂占所述改性铝合金熔体总量的0.4-0.6wt％，所述稀土金属：锶：钛或钛硼总量的质量比为1:(0.1-1.2)：(0.1-1.2)。The preparation method according to claim 1, characterized in that, the modifier accounts for 0.4-0.6wt% of the total amount of the modified aluminum alloy melt, and the total amount of the rare earth metal: strontium: titanium or titanium boron The mass ratio is 1:(0.1-1.2):(0.1-1.2).
  8. 根据权利要求1所述的制备方法，其特征在于，所述步骤S5中，所述固溶处理中的升温速率控制在1.5-3℃/min，保温时间控制在120-180min。The preparation method according to claim 1, characterized in that, in the step S5, the heating rate in the solution treatment is controlled at 1.5-3° C./min, and the holding time is controlled at 120-180 min.
  9. 根据权利要求1所述的制备方法，其特征在于，所述固溶处理、所述淬水处理、以及所述时效处理为连续处理，The preparation method according to claim 1, characterized in that, the solution treatment, the quenching treatment, and the aging treatment are continuous treatment,
    且所述水浴为循环水浴，所述淬水处理后，在进行所述时效处理前所述铸造铝合金素坯的温度保持在55℃以上。In addition, the water bath is a circulating water bath. After the water quenching treatment, the temperature of the cast aluminum alloy biscuit is kept above 55° C. before the aging treatment.
  10. 根据权利要求1所述的制备方法，其特征在于，所述时效处理阶段，从110-140℃以2-4℃/min的升温速率升温至160-200℃，此后自然冷却至室温。The preparation method according to claim 1, characterized in that in the aging treatment stage, the temperature is raised from 110-140°C to 160-200°C at a rate of 2-4°C/min, and then naturally cooled to room temperature.
  11. 一种高塑性复合改性铝合金制件，其特征在于，根据权利要求1至10任一项所述的制备方法制备得到，所述高塑性复合改性铝合金制件的抗拉强度为280MPa以上，屈服强度为200MPa以上，延伸率为12％以上。A high-plastic composite modified aluminum alloy product, characterized in that it is prepared according to the preparation method described in any one of claims 1 to 10, and the tensile strength of the high-plastic composite modified aluminum alloy product is 280MPa Above, the yield strength is 200 MPa or more, and the elongation is 12% or more.
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