CN114277272A - Composite rare earth alloy for modifying aluminum alloy and preparation method thereof - Google Patents
Composite rare earth alloy for modifying aluminum alloy and preparation method thereof Download PDFInfo
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- CN114277272A CN114277272A CN202111615720.5A CN202111615720A CN114277272A CN 114277272 A CN114277272 A CN 114277272A CN 202111615720 A CN202111615720 A CN 202111615720A CN 114277272 A CN114277272 A CN 114277272A
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Abstract
The invention provides a composite rare earth alloy for modifying aluminum alloy and a preparation method thereof. The preparation method comprises the following steps: step S1, providing an aluminum melt; step S2, providing an alterant, a refiner 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; and step S3, adding the alterant, the refiner and the rare earth aluminum alloy into the aluminum melt in an inert gas atmosphere, and smelting to obtain the composite rare earth alloy for modifying the aluminum alloy. According to the preparation method of the composite rare earth alloy for modifying the aluminum alloy, disclosed by the embodiment of the invention, by introducing the rare earth metal, the mutual poisoning effect between the modifier and the refiner is greatly overcome, the addition amounts of the modifier and the refiner can be increased, and the modification and refinement effects can be improved.
Description
Technical Field
The invention relates to the technical field of alloy materials and preparation, in particular to a composite rare earth alloy for modifying aluminum alloy and a preparation method thereof.
Background
Nowadays, the mechanical properties such as strength, yield strength, elongation and the like of the cast aluminum alloy commonly used in the market are not high enough, so that the problem of lightening and thinning the cast aluminum alloy parts is bottleneck. As an aerospace and transportation tool, the parts of the aerospace and transportation tool are required to have higher comprehensive mechanical properties on the premise of reducing the overall weight.
The aluminum alloy has the advantages of light weight, wear resistance, low thermal expansion coefficient, good casting performance, optimal matching relation of product mechanical properties (optimality of strength and plasticity) and the like, and is mainly composed of alpha-Al dendrites, eutectic silicon and Mg2Si equilibrium phase. However, under as-cast conditions, the coarse α -Al dendrites and the flaky and massive eutectic silicon severely deteriorate the mechanical properties, especially the plasticity and tensile strength, and limit the practical industrial application thereof.
In the prior art, an aluminum-titanium and aluminum-titanium-boron intermediate alloy series is used as a refiner, and an aluminum-strontium intermediate alloy is used as a modifier to refine and modify the aluminum alloy. However, when the Sr-containing alterant and the B-containing refiner are used simultaneously, mutual poisoning between Sr and B is easy to occur, and the effects of alteration and refinement are reduced (refer to Liaocheng, Sunpong; study on reaction products between Sr and B in cast Al-Si alloy; Metallurgical journal, 2003, 39(2): 155-. Therefore, the mechanical properties of the cast aluminum alloy are still difficult to meet the use requirements.
Therefore, it is highly desirable to provide a composite rare earth alloy for modifying aluminum alloy and a method for preparing the same, which can further improve the mechanical properties of cast aluminum alloy and improve the modification and refinement effects.
Disclosure of Invention
In view of the above, the present invention provides a composite rare earth alloy for modifying aluminum alloy, which can further improve the mechanical properties of cast aluminum alloy and improve the modification and refinement effects, and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the composite rare earth alloy for modifying the aluminum alloy according to the embodiment of the first aspect of the invention comprises the following steps:
step S1, providing an aluminum melt;
step S2, providing an alterant, a refiner 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;
and step S3, adding the alterant, the refiner and the rare earth aluminum alloy into the aluminum melt in an inert gas atmosphere, and smelting to obtain the composite rare earth alloy for modifying the aluminum alloy.
According to some embodiments of the invention, the step S1 includes:
step S11, providing an aluminum ingot;
step S12, removing an oxide skin layer on the surface of the aluminum ingot;
step S13, cleaning and drying the aluminum ingot with the oxide layer removed;
step S14, smelting the dried aluminum ingot to obtain an initial melt;
and step S15, refining the initial melt to obtain the aluminum melt.
According to some embodiments of the invention, the preparation of the rare earth aluminum alloy comprises the steps of:
adding the rare earth metal or the intermediate alloy containing the rare earth metal into the aluminum melt under inert atmosphere, and stirring the mixture to be completely molten while heating the mixture;
after the materials are completely melted, continuously preserving the heat for 10 to 20 minutes to homogenize the materials;
refining the homogenized melt;
and standing for a preset time after refining, and pouring to obtain the rare earth aluminum alloy.
According to some embodiments of the invention, the modifier is an aluminum strontium master alloy and the refiner is an aluminum titanium master alloy or an aluminum titanium boron master alloy.
Wherein the aluminum melt accounts for 86-88 wt%, the aluminum-strontium intermediate alloy accounts for 5.5-6.5 wt%, the aluminum-titanium or aluminum-titanium-boron intermediate alloy accounts for 0.1-0.2 wt%, and the rare earth aluminum alloy (such as Al-10La, Al-20La, Al-10Ce, Al-20Ce, Al-10Y or Al-20Y) accounts for 6.5-7.5 wt% of the total weight of the composite rare earth alloy for modifying the aluminum alloy.
Further, the modifier and/or the refiner and/or the rare earth aluminum alloy are respectively subjected to scale layer removal, ultrasonic cleaning and refining treatment in sequence.
Further, in step S3, the modifier is added separately from the refiner, and the rare earth aluminum alloy is added before the modifier and the refiner, or together with the first one, or in the gap between the modifier and the refiner.
According to some embodiments of the invention, the step S3 includes:
step S301, adding the rare earth aluminum alloy into the aluminum melt and smelting to obtain a first uniform mixed melt;
step S302, adding the alterant into the first uniformly mixed melt and continuously smelting to obtain a second uniformly mixed melt;
step S303, adding the refiner into the second uniformly mixed melt and continuously smelting to obtain the composite rare earth alloy.
Further, the step S301 includes:
heating the aluminum melt to 780-820 ℃ in an argon atmosphere, and adding the rare earth aluminum alloy;
after the rare earth aluminum alloy is completely melted, continuously stirring for 5-15 minutes to carry out homogenization treatment;
after the homogenization treatment, standing and preserving heat for 5-20 minutes for heat preservation treatment;
and refining after the heat preservation treatment is finished to obtain the first uniformly mixed melt.
According to further embodiments of the present invention, the step S3 includes:
step S311, adding the rare earth aluminum alloy and the alterant into the aluminum melt at the same time, and continuously smelting to obtain a third uniform mixed melt;
and S312, adding the refiner into the third uniformly mixed melt and continuously smelting to obtain the composite rare earth alloy.
Further, after the third uniformly mixed melt is obtained, the third uniformly mixed melt is refined, and the refiner is added after the third uniformly mixed melt is refined.
According to further embodiments of the present invention, the step S3 includes:
step S321, adding the alterant into the aluminum melt and continuously smelting to obtain a fourth uniformly mixed melt;
step S322, adding the rare earth aluminum alloy into the fourth uniformly mixed melt and continuously smelting to obtain a fifth uniformly mixed melt;
and S323, adding the refiner into the fifth uniformly mixed melt and continuously smelting to obtain the composite rare earth alloy.
Further, the fourth homogeneous mixed melt and the fifth homogeneous mixed melt are refined respectively, and the next step is executed after refining.
According to some embodiments of the invention, the refining comprises:
blowing the refining agent through inert gas and keeping for 3-10 minutes, adding deslagging agent and stirring for 5-10 minutes, and removing the surface scum.
Furthermore, the adding amount of the refining agent accounts for 0.1-0.3% of the mass of the added melt, and the adding amount of the slag removing agent accounts for 0.1-0.3% of the mass of the added melt;
the refining agent comprises the following components in percentage by mass:
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 and 8-12 parts of hexachloroethane;
the slag remover comprises the following components in percentage by mass:
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 fluosilicate, 5-10 parts of calcium fluoride, 1-5 parts of potassium nitrate and 5-10 parts of potassium fluosilicate.
Further, the density of the melt was measured before and during the refining, when the density of the melt was less than 2.65g/cm3If so, carrying out the refining treatment; when the melt density is more than or equal to 2.65g/cm3I.e., not performing the refining process or terminating the refining process.
The composite rare earth alloy for modifying an aluminum alloy according to the embodiment of the second aspect of the present invention contains strontium, titanium or titanium boron, and a rare earth metal, wherein in the composite rare earth alloy, the ratio of the rare earth metal: strontium: the mass ratio of the total amount of titanium or titanium boron is 1 (0.1-1.2): (0.1-1.2), and the rare earth metal is one or more selected from lanthanum, cerium and yttrium.
The technical scheme of the invention at least has one of the following beneficial effects:
according to the preparation method of the composite rare earth alloy for modifying the aluminum alloy, disclosed by the embodiment of the invention, by introducing the rare earth metal, the mutual poisoning effect between the modifier and the refiner is greatly overcome, the addition amounts of the modifier and the refiner can be increased, and the modification and refinement effects can be improved;
furthermore, the invention enables the modifier and the refiner to be added at intervals by reasonably adjusting the process, and the rare earth metal is added before the latter is added, so that the mutual poisoning between the modifier and the refiner can be further effectively avoided, and the modification and refinement effects can be further improved;
furthermore, the melt in each stage is refined to remove impurities, so that the mechanical property of the final aluminum alloy product is further improved.
Drawings
FIG. 1 is a metallographic structure image of an aluminum alloy before modification;
fig. 2 is a metallographic structure image of an aluminum alloy modified with the composite rare earth alloy prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, 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 with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention, are within the scope of the invention.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The use of "first," "second," and similar terms in the present application do not denote any order, quantity, or importance, but rather the terms are used to distinguish one element from another. Also, the use of the terms "a" or "an" and the like do not denote a limitation of quantity, but rather denote the presence of at least one.
The method for producing the composite rare earth alloy for modifying an aluminum alloy according to the embodiment of the present invention will be described first in detail.
The preparation method of the composite rare earth alloy for modifying the aluminum alloy, provided by the embodiment of the invention, comprises the following steps of:
step S1, providing an aluminum melt.
That is, an aluminum melt is first prepared.
Here, a commercially available high-purity aluminum ingot may be directly heated and melted to prepare an aluminum melt, or the aluminum ingot may be further purified. The purification treatment may, for example, comprise the following steps:
step S11, providing an aluminum ingot;
step S12, removing an oxide skin layer on the surface of the aluminum ingot;
step S13, cleaning and drying the aluminum ingot with the oxide layer removed;
step S14, smelting the dried aluminum ingot to obtain an initial melt;
and step S15, refining the initial melt to obtain the aluminum melt.
That is, for an aluminum ingot, an oxide skin layer on the surface thereof is first removed, thereafter, cleaning is performed to remove surface floating chips, melting is performed after drying, and the melt is refined. Details regarding the specific refining process will be described later.
After the above purification treatment, undesired impurities such as Fe, oxides, etc. can be removed therefrom. Is favorable for further improving the modification and refinement of the composite rare earth alloy.
It should be noted that, regarding Fe and its oxide, it can be removed by adding manganese or aluminum-manganese alloy to form surface scum, for example.
Step S2, providing an alterant, a refiner 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.
The modifier can be an aluminum-strontium intermediate alloy, and the refiner can be an aluminum-titanium intermediate alloy or an aluminum-titanium-boron intermediate alloy. That is, conventional modifiers and refiners may be used.
Further, as the modifier and/or the refiner, commercially available materials such as commercially available aluminum strontium master alloy, aluminum titanium boron master alloy, and the like; or the alloy can be prepared by respectively weighing corresponding metals of strontium, titanium and boron, and melting the metals in an aluminum melt to form a uniform alloy. With respect to the amounts of the modifier and the refiner, the amounts of the rare earth to be introduced and the specific composition of the aluminum alloy to be modified can be designed accordingly. Preferably, in terms of rare earth metals: strontium: the mass ratio of the total amount of titanium or titanium boron is 1 (0.1-1.2): (0.1-1.2) designing.
In addition, as the rare earth metal in the rare earth aluminum alloy, a group IIIB element having an electronic structure intervening therebetween may be selected in consideration of strontium in the modifier and titanium and boron in the refiner. Considering stability, resources and the like, it is preferable to use yttrium, one or more of lanthanum and cerium in lanthanide metals.
The rare earth aluminum alloy can be prepared, for example, by the following method:
adding the rare earth metal or the intermediate alloy containing the rare earth metal into the aluminum melt under inert atmosphere, and stirring the mixture to be completely molten while heating the mixture;
after the materials are completely melted, continuously preserving the heat for 10 to 20 minutes to homogenize the materials;
refining the homogenized melt;
and standing for a preset time after refining, and pouring to obtain the rare earth aluminum alloy.
As the alloy containing the rare earth metal, one or more commercially available Al-10Ce, Al-20La, Al-10La and Al-20Y, Al-10Y can be used, for example.
In addition, for the commercial aluminum strontium intermediate alloy, aluminum titanium intermediate alloy or aluminum titanium boron intermediate alloy, rare earth aluminum alloy, respectively, the descaling, ultrasonic cleaning and refining treatment can be sequentially carried out. Thereby, the undesirable impurities and oxides can be further removed, and the refining and modification effects of the composite rare earth alloy as a product can be improved.
And step S3, adding the alterant, the refiner and the rare earth aluminum alloy into the aluminum melt in an inert gas atmosphere, and smelting to obtain the composite rare earth alloy for modifying the aluminum alloy.
That is, after preparing the aluminum melt, the alterant, the refiner and the rare earth aluminum alloy are added into the aluminum melt for further smelting under the inert gas atmosphere, and the composite rare earth aluminum alloy is obtained.
According to the preparation method of the composite rare earth alloy for modifying the aluminum alloy, disclosed by the embodiment of the invention, by introducing the rare earth metal, the mutual poisoning effect between the modifier and the refiner is greatly overcome, the addition amounts of the modifier and the refiner can be increased, and the modification and refinement effects can be improved.
In addition, the inventors of the present invention have repeatedly studied and found that by adjusting the order of adding the modifying agent, the refining agent, and the rare earth aluminum alloy, the mutual poisoning between the modifying agent and the refining agent can be further effectively avoided, which is advantageous for further improving the modifying and refining effects.
Specifically, in step S3, the modifier is added to the alloy ingot at a distance from the refiner, and the rare earth aluminum alloy is added before the modifier and the refiner, or together with the first modifier, or at a distance from the modifier and the refiner. Therefore, the poisoning effect of strontium and boron/titanium can be effectively overcome, and the modification and refinement effects can be further improved.
Preferably, the step S3 can adopt the following three specific embodiments:
the first implementation mode comprises the following steps:
according to some embodiments of the invention, the step S3 includes:
step S301, adding the rare earth aluminum alloy into the aluminum melt and smelting to obtain a first uniform mixed melt;
step S302, adding the alterant into the first uniformly mixed melt and continuously smelting to obtain a second uniformly mixed melt;
step S303, adding the refiner into the second uniformly mixed melt and continuously smelting to obtain the composite rare earth alloy.
That is, in the present embodiment, the rare earth aluminum alloy is first added, and thereafter, the modifier and the refiner are added in this order.
Further, the step S301 includes:
heating the aluminum melt to 780-820 ℃ in an argon atmosphere, and adding the rare earth aluminum alloy;
after the rare earth aluminum alloy is completely melted, continuously stirring for 5-15 minutes to carry out homogenization treatment;
after the homogenization treatment, standing and preserving heat for 5-20 minutes for heat preservation treatment;
and refining after the heat preservation treatment is finished to obtain the first uniformly mixed melt.
The second embodiment:
according to further embodiments of the present invention, the step S3 includes:
step S311, adding the rare earth aluminum alloy and the alterant into the aluminum melt at the same time, and continuously smelting to obtain a third uniform mixed melt;
and S312, adding the refiner into the third uniformly mixed melt and continuously smelting to obtain the composite rare earth alloy.
That is, in the present embodiment, first, the rare earth aluminum alloy is added together with the aluminum-strontium intermediate alloy as the modifier, and after it is completely melted and homogenized, the refiner is added thereto.
Further, after the third uniformly mixed melt is obtained, the third uniformly mixed melt is refined, and the refiner is added after the third uniformly mixed melt is refined.
The third embodiment is as follows:
according to further embodiments of the present invention, the step S3 includes:
step S321, adding the alterant into the aluminum melt and continuously smelting to obtain a fourth uniformly mixed melt;
step S322, adding the rare earth aluminum alloy into the fourth uniformly mixed melt and continuously smelting to obtain a fifth uniformly mixed melt;
and S323, adding the refiner into the fifth uniformly mixed melt and continuously smelting to obtain the composite rare earth alloy.
That is, in the present embodiment, the modifier is first added, the rare earth aluminum alloy is added after completely melting and homogenizing, and the aluminum-titanium intermediate alloy/aluminum-titanium-boron intermediate alloy as the refiner is finally added after further completely melting and homogenizing.
Further, the fourth homogeneous mixed melt and the fifth homogeneous mixed melt are refined respectively, and the next step is executed after refining.
Further, the refining in any of the above steps, i.e., the refining in the purification process of the aluminum melt, the refining in the preparation process of the rare earth aluminum alloy, and the refining of each melt in step S3, may be performed in the following manner:
the refining comprises the following steps:
blowing the refining agent through inert gas and keeping for 3-10 minutes, adding deslagging agent and stirring for 5-10 minutes, and removing the surface scum.
Furthermore, the adding amount of the refining agent accounts for 0.1-0.3% of the mass of the added melt, and the adding amount of the slag removing agent accounts for 0.1-0.3% of the mass of the added melt;
the refining agent comprises the following components in percentage by mass:
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 and 8-12 parts of hexachloroethane;
the slag remover comprises the following components in percentage by mass:
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 fluosilicate, 5-10 parts of calcium fluoride, 1-5 parts of potassium nitrate and 5-10 parts of potassium fluosilicate.
Further, the density of the melt was measured before and during the refining, when the density of the melt was less than 2.65g/cm3If so, carrying out the refining treatment; when the melt density is more than or equal to 2.65g/cm3I.e., not performing the refining process or terminating the refining process.
In practice, the hydrogen content is estimated by measuring the density of the melt, and it is generally accepted that the higher the density the lower the hydrogen content, as a standard when the density reaches 2.65g/cm3The hydrogen content can be considered to reach the standard without further refining. Of course, for higher quality requirements, the density standard may also be set to 2.67g/cm3Or higher.
The composite rare earth alloy for modifying an aluminum alloy according to the embodiment of the second aspect of the present invention contains strontium, titanium or titanium boron, and a rare earth metal, wherein 1 (0.1-1.2): (0.1-1.2), and the rare earth metal is one or more selected from lanthanum, cerium and yttrium.
The production process according to the present invention is further illustrated in detail by the following specific examples.
Example 1
1) Preparation of aluminium melt
Raw materials: high purity aluminum ingot (purchased from medium aluminum group, composition: Al (99.99%), Fe < 0.1%, impurity < 0.05%)
Refining agent:
the components: 15 parts of potassium chloride, 20 parts of sodium chloride, 210 parts of CaF, 320 parts of Na2CO, 410 parts of Na2SO, 615 parts of Na3AlF and 610 parts of C2Cl
Deslagging agent:
the components: 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 fluosilicate, 10 parts of calcium fluoride, 5 parts of potassium nitrate and 10 parts of potassium fluosilicate
Pretreatment: and (4) cleaning the oxide skin and the surface layer on the surface of the high-purity aluminum by using a grinding wheel machine.
Ultrasonic cleaning: and (4) putting the pretreated high-purity aluminum ingot into a cleaning agent for ultrasonic treatment.
Drying: and (3) placing the high-purity aluminum ingot subjected to ultrasonic cleaning into a baking oven furnace, and baking for 30-60 minutes at the temperature of 60-100 ℃.
Smelting: and putting the dried high-purity aluminum into a preheated crucible, and heating and melting at 760 and 800 ℃.
Refining treatment: and refining after the high-purity aluminum is melted. Specifically, the method comprises the following steps: and refining the molten high-purity aluminum by using an Ar + graphite automatic degassing stirring rod. Blowing Ar into the melt for refining at 740-760 ℃ for 5-10 min, wherein the refining dose is 0.1-0.3%, and keeping the temperature for 3-5 min. And standing for 10-20 minutes, and adding 0.1-0.3% of deslagging agent into the mixture to uniformly disperse the deslagging agent, and removing the surface scum.
Standing: standing for 8-15 minutes at 740-760 ℃ after slagging off.
2) Preparation of high-purity rare earth aluminum alloy
Melting and processing the rare earth alloy: adjusting the temperature of the high-purity aluminum obtained in the step 1) to 780-820 ℃, heating to completely melt the high-purity aluminum, and adding a rare earth aluminum lanthanum alloy (purchased from Baotou rare earth research institute, components: al-10La, Fe <0.05, impurity content less than or equal to 0.15). Heating at 780-820 ℃ under the protection of argon atmosphere to completely melt the alloy.
Stirring and heat preservation: stirring the melted melt for 3-5 min to homogenize the melt, and maintaining the temperature of the melt at 760-780 ℃ for 10-20 min.
Refining treatment: the whole process is carried out under the protection of argon atmosphere, and refining treatment is carried out after the rare earth aluminum lanthanum alloy is melted. And introducing an Ar + graphite automatic degassing stirring rod to refine the molten graphite. Blowing Ar into the refining agent at 780 ℃ for 5-10 minutes, wherein the refining agent is 0.3 wt% of melt, and boiling bubbles cannot be formed on the upper surface of the molten aluminum in the refining process. Removing scum on the surface of the melt: after refining for 15-20 minutes, 0.2 wt% of deslagging agent is added to be uniformly dispersed, and scum on the surface is removed.
Standing: standing for 10-15 minutes at 720-730 ℃ after slagging off.
Casting: and (3) quickly casting the melt in a mould to ensure that all components are uniform. The process adopts full water cooling to cool the device.
3) Refining treatment of Al-Sr intermediate alloy and Al-Ti-B intermediate alloy
3.1) aluminum-strontium master alloy: from Nantong-Onshi Metal materials Ltd, composition: al-10Sr, Fe <0.05, and impurity content less than or equal to 0.15.
Pretreatment: and (3) cleaning the oxide skin and the surface layer of the aluminum-strontium intermediate alloy by using a grinding wheel machine.
Ultrasonic cleaning: and (3) putting the pretreated aluminum-strontium intermediate alloy into an ultrasonic cleaning tank for ultrasonic treatment.
Drying: and (3) putting the cleaned aluminum-strontium intermediate alloy into an oven furnace, and baking for 30-60 minutes at the temperature of 60-100 ℃.
Smelting: the aluminum-strontium intermediate alloy is put into a preheated crucible to be melted at 760-780 ℃.
Refining treatment: and refining after the aluminum-strontium intermediate alloy is melted. And introducing an Ar + graphite automatic degassing stirring rod to refine the molten high-purity aluminum. Blowing Ar into the molten aluminum for refining at the temperature of 730-750 ℃ for 5-10 minutes, wherein the blowing refining dose is 0.1-0.3 percent of the melt, and keeping the melt for 3-5 minutes, and no boiling bubbles can be formed on the upper surface of the molten aluminum in the refining process.
Removing surface scum: and (3) putting 0.1-0.3% of deslagging agent into the mixture for 15-20 minutes, uniformly dispersing, and removing the scum on the surface.
Standing: standing for 8-15 minutes at 740-760 ℃ after slagging off.
3.2) aluminum titanium boron intermediate alloy: from Nantong Angshen Metal materials Co., Ltd (composition and content: Ti: 5%, B: 1%, remainder: Al)
The aluminum titanium boron intermediate alloy as the refiner was treated in the same manner as described above.
4) Preparation of composite rare earth alloy
Respectively preparing an aluminum melt, a rare earth aluminum alloy, an aluminum strontium intermediate alloy and an aluminum titanium boron intermediate alloy through the steps of 1) to 3), and then carrying out mixed smelting on the aluminum melt, the rare earth aluminum alloy, the aluminum strontium intermediate alloy and the aluminum titanium boron intermediate alloy to obtain the composite rare earth alloy serving as a product.
In this embodiment, as the order of addition, the rare earth aluminum alloy is added to the aluminum melt, followed by the aluminum-strontium alloy, and finally the aluminum-titanium alloy. The method comprises the following specific steps:
step 1, batching: weighing the obtained high-purity aluminum, the aluminum-titanium-boron intermediate alloy, the aluminum-strontium intermediate alloy and the rare earth aluminum alloy according to the required mass percentage, and then preheating.
Based on 100 parts of total weight, high-purity aluminum: 4.8 parts of aluminum-titanium-boron intermediate alloy: 0.2 part of aluminum-strontium intermediate alloy: 60 parts of rare earth aluminum alloy: 35 portions of
Step 2, adding and melting rare earth aluminum alloy: for the aluminum melt, firstly heating the rare earth aluminum alloy to 780-820 ℃ to soften the aluminum alloy before melting, then controlling the overall temperature of the aluminum melt to 760-780 ℃, and adding the rare earth aluminum alloy into the aluminum melt for heat preservation.
The whole process adopts argon atmosphere protection to melt rare earth aluminum alloy.
And 3, after the rare earth aluminum alloy is completely melted, controlling the temperature to be 750-770 ℃, and stirring for 5-10 minutes.
The whole process adopts argon atmosphere for protection, and the stirring rod adopts graphite material and is preheated to 400-plus-500 ℃ before stirring.
That is, after the rare earth aluminum alloy is completely melted, the temperature is slightly lowered, and it is possible to prevent subsequent grain coarsening and the like due to overheating.
And 4, performing heat preservation treatment on the melted melt at 740-760 ℃ for 5-20 minutes. In this stage, an alloying reaction occurs.
And 5, refining: after the heat preservation is finished, refining, degassing and deslagging are carried out. Blowing 0.3% of refining agent into the melt through argon, and controlling the ventilation time to be 3-8 minutes; then, the mixture was further added to 0.2% of a slag remover, stirred for 5 minutes, allowed to stand and removed of slag and impurities on the surface layer of the melt. The whole process adopts argon atmosphere protection.
The aluminum melt was sampled before and during refining and its density was measured to estimate the hydrogen content. The measurement method adopts a density method (with the theoretical value of aluminum being 2.70 g/cm)3For comparison), the closer the measured sample is to 2.7g/cm3The lower the internal hydrogen content of the aluminum. Generally, the normal rate is less than 2.7g/cm3(ii) a The density of the sample is measured to be approximately equal to 2.65g/cm3The hydrogen content can be estimated by vacuumizing, and if the hydrogen content is unqualified, refining is further carried out, namely, the refining agent is repeatedly added and the slag removing agent is refined again.
Step 6, standing: and standing the melt which is added with the rare earth aluminum alloy and refined for 3-5 minutes, and controlling the temperature at 740-760 ℃.
And 7, adding and melting an aluminum-strontium intermediate alloy: and (3) adding the refined aluminum-strontium intermediate alloy into the melt obtained in the step (6), and controlling the temperature to be 780-820 ℃ so that the aluminum-strontium intermediate alloy is completely melted. The whole process adopts argon atmosphere protection to melt the aluminum-strontium intermediate alloy.
And 8, after the aluminum-strontium intermediate alloy is melted, controlling the temperature to be 740-760 ℃, and stirring for 3-8 minutes to realize homogenization. The whole process adopts argon atmosphere for protection, the stirring rod adopts graphite material, and the stirring rod is preheated to 400-plus-500 ℃ before stirring.
And 9, performing heat preservation treatment at 725-750 ℃. The heat preservation time is controlled to be 15-30 minutes.
Step 10, refining, degassing and deslagging: after the heat preservation of the melt is finished, blowing argon gas into the melt, and then blowing 0.3% of refining agent into the aluminum-rare earth composite melt, wherein the ventilation time is controlled to be 5-10 minutes; adding 0.2% of slag skimming agent into the aluminum melt, stirring for 5 minutes and fishing out slag and impurities on the surface layer of the aluminum-rare earth composite melt. The whole process adopts argon atmosphere protection.
The aluminum melt was sampled before and during refining to determine the hydrogen content. (hydrogen content required: 2.65g/cm or more3(ii) a ) Vacuumizing in the hydrogen measuring process, and further refining if the hydrogen content is unqualified, namely, repeatedly adding a refining agent and removing slagThe agent is refined again.
Step 11, adding an aluminum-titanium-boron intermediate alloy: and (3) adding an aluminum-titanium-boron intermediate alloy into the melt treated in the step (10), heating to completely melt the aluminum-titanium-boron intermediate alloy, and uniformly stirring for 3-5 minutes to homogenize the aluminum-titanium-boron intermediate alloy.
Step 12, heat preservation: after stirring, the melt is kept at the temperature of 715-725 ℃ for 8-12 minutes.
Step 13, refining, degassing and deslagging: after the heat preservation of the melt is finished, blowing argon gas into the melt, and then blowing 0.3% of refining agent into the aluminum-rare earth composite melt, wherein the ventilation time is controlled to be 5-10 minutes; adding 0.2% of slag skimming agent into the aluminum melt, stirring for 5 minutes and fishing out slag and impurities on the surface layer of the aluminum-rare earth composite melt. The whole process adopts argon atmosphere protection.
The aluminum melt was sampled before and during refining to determine the hydrogen content. (hydrogen content required: 2.65g/cm or more3(ii) a ) And (3) vacuumizing in the hydrogen measuring process, and if the hydrogen content is unqualified, further refining, namely repeatedly adding a refining agent and a deslagging agent, and refining again until the hydrogen content is qualified.
Step 14, casting: the mold was preheated at 300 ℃ to 400 ℃. And (3) controlling the temperature of the composite rare earth alloy melt obtained in the step (13) to be 715-725 ℃ for casting.
Preferably, during casting, the oxide on the surface layer of the aluminum-rare earth composite melt is filtered by a filter screen of glass fiber; and filtering the surface layer of the aluminum-rare earth composite melt before each casting, and then casting.
Preferably, the cooling control of the cast mould is that the aluminum rare earth composite melt cast into the mould is cooled in a water cooling mode, the solidification speed of the aluminum melt is controlled at 50-100 ℃/s in the cooling process, and the solidification mode is sequentially solidified.
The composite rare earth aluminum alloy obtained in the above embodiment is prepared by adding rare earth aluminum alloy and adjusting the adding sequence, and according to some embodiments of the invention, the rare earth metal: strontium: the mass ratio of the titanium or the titanium boron is 1 (0.1-1.2): (0.1-1.2). That is, the content of the modifier and the refiner can be increased and the modifier and the refiner can sufficiently function.
In addition, the aluminum alloy is modified by using the composite rare earth aluminum alloy obtained in the embodiment. Fig. 1 shows the metallographic structure of an aluminum alloy before modification, and fig. 2 shows the metallographic structure after modification. As can be seen from fig. 1 and 2, the metallographic structure of the aluminum alloy before modification (fig. 1) shows that the coarse primary α -Al phase is in the form of dendrite structure, and the diameter, length, and dendrite spacing of the secondary dendrites are relatively large. The metallographic structure of the improved aluminum alloy has a large amount of rosette alpha-Al phase and round spherical alpha-Al phase, the primary alpha-Al phase is obviously refined, and the number of dendritic crystals is reduced. That is, after modification, the crystal grains are sufficiently refined and the microstructure is uniform.
In addition, mechanical properties of a356 aluminum alloy modified with the composite rare earth aluminum alloy obtained in this example were evaluated. The evaluation results (described as example 1) are shown in table 1 below. For comparison, the results of the tests on the unmodified A356 aluminum alloy (before modification) are also shown. Meanwhile, the test results of the A356 aluminum alloy modified by adding the modifier and the refiner in the same proportion are shown in place of the composite rare earth aluminum alloy of the embodiment (marked as comparative example 1).
TABLE 1A 356 aluminum alloy and modified mechanical Property test results
| Mechanical Properties | Before modification | Comparative example 1 | Example 1 |
| Tensile strength (MPa) | 125-145 | 175-190 | 205-210 |
| Yield strength (MPa) | 65-80 | 85-95 | 100-115 |
| Elongation (%) | 3-5 | 6-8 | 10-12 |
As can be seen from table 1, by using the composite rare earth aluminum alloy of the present example, the elongation, yield strength, and tensile strength were greatly improved, and the comprehensive mechanical properties were greatly improved.
Example 2
In this example, the same as example 1 except that the aluminum-strontium master alloy was added together with the rare earth aluminum alloy.
In the following, only the parts involved in the preparation of the composite rare earth alloy are described as follows:
4) preparation of composite rare earth alloy
Step 1, batching: weighing the obtained high-purity aluminum, the aluminum-titanium-boron intermediate alloy, the aluminum-strontium intermediate alloy and the rare earth aluminum alloy according to the required mass percentage, and then preheating.
Taking 100 parts as an example, high-purity aluminum: 4.8 parts of aluminum-titanium-boron intermediate alloy: 0.2 part of aluminum-strontium intermediate alloy: 60 parts of rare earth aluminum alloy: 35 portions of
Step 2, adding and melting rare earth aluminum alloy and aluminum-strontium intermediate alloy: and (3) controlling the temperature of the aluminum melt to be 760-780 ℃, and adding the rare earth alloy material and the aluminum-strontium intermediate alloy into the aluminum melt.
The whole process adopts argon atmosphere protection, and the rare earth aluminum alloy is melted when the temperature is controlled to be 780-820 ℃.
And 3, after the rare earth aluminum alloy and aluminum-strontium intermediate alloy is completely melted, controlling the temperature to be 750-770 ℃, and stirring for 10 minutes. The whole process adopts argon atmosphere protection, the stirring rod adopts graphite material, and the temperature is preheated to 450 ℃ before stirring.
And 4, performing heat preservation treatment on the melted melt at 740-760 ℃ for 10 minutes.
And 5, refining: after the heat preservation is finished, refining, degassing and deslagging are carried out. Blowing 0.3 wt% of refining agent into the melt through argon, and controlling the aeration time to be 5 minutes; thereafter, 0.2 wt% of a slag remover was further added, stirred for 5 minutes, and left to stand to remove slag and impurities on the surface layer of the melt. The whole process adopts argon atmosphere protection.
The aluminum melt was sampled before and during refining to estimate the hydrogen content. (required melt density: 2.65g/cm or more)3. ) And (3) vacuumizing in the hydrogen measuring process, and further refining if the hydrogen content is unqualified, namely, repeatedly adding a refining agent and a deslagging agent for refining again.
Step 6, standing: and standing the melt which is added with the rare earth aluminum alloy and refined for 3-5 minutes, and controlling the temperature at 740-760 ℃.
Thereafter, an aluminum-titanium-boron intermediate alloy is further added to the alloy and melted. The specific steps can be referred to in example 1, and detailed description thereof is omitted here.
In addition, the experimental result shows that the composite rare earth aluminum alloy obtained according to the embodiment can also effectively improve the mechanical strength of the aluminum alloy and realize better refining and modification effects. The detailed data thereof is omitted here.
Example 3
In this example, the same as in example 1, except that the rare earth aluminum alloy was added after the aluminum-strontium alloy was added.
In the following, only the parts involved in the preparation of the composite rare earth alloy are described as follows:
4) preparation of composite rare earth alloy
Step 1, adding and melting an aluminum-strontium intermediate alloy: and adding the refined aluminum-strontium intermediate alloy into an aluminum melt, and controlling the temperature to be 780-820 ℃ so that the aluminum-strontium intermediate alloy is completely melted. The whole process adopts argon atmosphere protection to melt the aluminum-strontium intermediate alloy.
And 2, after the aluminum-strontium intermediate alloy is melted, controlling the temperature to be 740-760 ℃, and stirring for 3-8 minutes to realize homogenization. The whole process adopts argon atmosphere for protection, the stirring rod adopts graphite material, and the stirring rod is preheated to 400-plus-500 ℃ before stirring.
And 3, performing heat preservation treatment at 725-750 ℃. The heat preservation time is controlled to be 15-30 minutes.
Step 4, refining, degassing and deslagging: after the heat preservation of the melt is finished, blowing argon gas into the melt, and then blowing 0.3 wt% of refining agent into the aluminum-rare earth composite melt, wherein the ventilation time is controlled to be 10 minutes; adding 0.2 wt% of slag removing agent into the aluminum melt, stirring for 5 minutes and fishing out slag and impurities on the surface layer of the aluminum-rare earth composite melt. The whole process adopts argon atmosphere protection.
The aluminum melt was sampled before and during refining to determine the hydrogen content. (hydrogen content required: 2.65g/cm or more3(ii) a ) And (3) vacuumizing in the hydrogen measuring process, and further refining if the hydrogen content is unqualified, namely, repeatedly adding a refining agent and a deslagging agent for refining again.
Step 5, adding and melting rare earth aluminum alloy: and (4) controlling the temperature of the melt in the step (4) to be 760-780 ℃, and adding the rare earth alloy material into the melt.
The whole process adopts argon atmosphere protection, and the rare earth aluminum alloy is melted when the temperature is controlled to be 780-820 ℃.
And 6, after the rare earth aluminum alloy is completely melted, controlling the temperature to be 750-770 ℃, and stirring for 10 minutes. The whole process adopts argon atmosphere for protection, the stirring rod adopts graphite material, and the stirring rod is preheated to 400-plus-500 ℃ before stirring.
And 7, performing heat preservation treatment on the melted melt at 740-760 ℃ for 10 minutes.
And 8, refining: after the heat preservation is finished, refining, degassing and deslagging are carried out. Blowing 0.3 wt% of refining agent into the melt through argon, and controlling the aeration time to be 5 minutes; then, the mixture was further added to 0.2 wt% of a slag remover, stirred for 5 minutes, allowed to stand and removed of slag and impurities on the surface layer of the melt. The whole process adopts argon atmosphere protection.
The aluminum melt was sampled before and during refining to estimate the hydrogen content. (required melt density: 2.65g/cm or more)3. ) And (3) vacuumizing in the hydrogen measuring process, and further refining if the hydrogen content is unqualified, namely, repeatedly adding a refining agent and a deslagging agent for refining again.
Step 9, standing: and standing the melt which is added with the rare earth aluminum alloy and refined for 3-5 minutes, and controlling the temperature at 740-760 ℃.
Thereafter, an aluminum-titanium-boron intermediate alloy is further added to the alloy and melted. The specific steps can be referred to in example 1, and detailed description thereof is omitted here.
In addition, the experimental result shows that the composite rare earth aluminum alloy obtained according to the embodiment can also effectively improve the mechanical strength of the aluminum alloy and realize better refining and modification effects. The detailed data thereof is omitted here.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (16)
1. The preparation method of the composite rare earth alloy for modifying the aluminum alloy is characterized by comprising the following steps of:
step S1, providing an aluminum melt;
step S2, providing an alterant, a refiner 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;
and step S3, adding the alterant, the refiner and the rare earth aluminum alloy into the aluminum melt in an inert gas atmosphere, and smelting to obtain the composite rare earth alloy for modifying the aluminum alloy.
2. The method for preparing a composite material according to claim 1, wherein the step S1 includes:
step S11, providing an aluminum ingot;
step S12, removing an oxide skin layer on the surface of the aluminum ingot;
step S13, cleaning and drying the aluminum ingot with the oxide layer removed;
step S14, smelting the dried aluminum ingot to obtain an initial melt;
and step S15, refining the initial melt to obtain the aluminum melt.
3. The method according to claim 1, wherein the preparation of the rare earth aluminum alloy comprises the steps of:
adding the rare earth metal or the intermediate alloy containing the rare earth metal into the aluminum melt under inert atmosphere, heating and stirring until the mixture is completely melted;
after the materials are completely melted, continuously preserving the heat for 10 to 20 minutes to homogenize the materials;
refining the homogenized melt;
and standing for a preset time after refining, and pouring to obtain the rare earth aluminum alloy.
4. The preparation method according to claim 1, wherein the modifier is an aluminum-strontium intermediate alloy, and the refiner is an aluminum-titanium intermediate alloy or an aluminum-titanium-boron intermediate alloy.
5. The method according to claim 4, wherein the modifier and/or the refiner and/or the rare earth aluminum alloy are sequentially subjected to descaling, ultrasonic cleaning and refining.
6. The production method according to claim 4, wherein in the step S3, the alterant is added separately from the refiner, and the rare earth aluminum alloy is added before the alterant and the refiner, or together with the first addition, or in the gap between the alterant and the refiner.
7. The method for preparing a composite material according to claim 6, wherein the step S3 includes:
step S301, adding the rare earth aluminum alloy into the aluminum melt and smelting to obtain a first uniform mixed melt;
step S302, adding the alterant into the first uniformly mixed melt and continuously smelting to obtain a second uniformly mixed melt;
step S303, adding the refiner into the second uniformly mixed melt and continuously smelting to obtain the composite rare earth alloy.
8. The method according to claim 7, wherein the step S301 includes:
heating the aluminum melt to 780-820 ℃ in an argon atmosphere, and adding the rare earth aluminum alloy;
after the rare earth aluminum alloy is completely melted, continuously stirring for 5-15 minutes to carry out homogenization treatment;
after the homogenization treatment, standing and preserving heat for 5-20 minutes for heat preservation treatment;
and refining after the heat preservation treatment is finished to obtain the first uniformly mixed melt.
9. The method for preparing a composite material according to claim 6, wherein the step S3 includes:
step S311, adding the rare earth aluminum alloy and the alterant into the aluminum melt at the same time, and continuously smelting to obtain a third uniform mixed melt;
and S312, adding the refiner into the third uniformly mixed melt and continuously smelting to obtain the composite rare earth alloy.
10. The method of claim 9, wherein the third intimately mixed melt is refined after it is obtained, and the refiner is added after refining.
11. The method for preparing a composite material according to claim 6, wherein the step S3 includes:
step S321, adding the alterant into the aluminum melt and continuously smelting to obtain a fourth uniformly mixed melt;
step S322, adding the rare earth aluminum alloy into the fourth uniformly mixed melt and continuously smelting to obtain a fifth uniformly mixed melt;
and S323, adding the refiner into the fifth uniformly mixed melt and continuously smelting to obtain the composite rare earth alloy.
12. The method of claim 11, wherein the fourth and fifth homogeneous mixed melts are refined separately, and the next step is performed after refining.
13. The method of any one of claims 2, 3, 5, 8, 10, and 12, wherein the refining comprises:
blowing the refining agent through inert gas and keeping for 3-10 minutes, adding deslagging agent and stirring for 5-10 minutes, and removing the surface scum.
14. The preparation method of the alloy material according to claim 13, wherein the addition amount of the refining agent accounts for 0.1-0.3% of the mass of the added melt, and the addition amount of the slag removing agent accounts for 0.1-0.3% of the mass of the added melt;
the refining agent comprises the following components in percentage by mass:
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 and 8-12 parts of hexachloroethane;
the slag remover comprises the following components in percentage by mass:
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 fluosilicate, 5-10 parts of calcium fluoride, 1-5 parts of potassium nitrate and 5-10 parts of potassium fluosilicate.
15. The method of claim 14, wherein the melt is tested for density before and during refining when the melt has a density of less than 2.65g/cm3If so, carrying out the refining treatment;
when the melt density is more than or equal to 2.65g/cm3I.e., not performing the refining process or terminating the refining process.
16. The composite rare earth alloy for modifying the aluminum alloy is characterized by comprising strontium, titanium or titanium boron and rare earth metals, wherein the weight ratio of the rare earth metals: strontium: the mass ratio of the total amount of titanium or titanium boron is 1 (0.1-1.2): (0.1-1.2), and the rare earth metal is one or more selected from lanthanum, cerium and yttrium.
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| CN115133012A (en) * | 2022-07-22 | 2022-09-30 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Coral-shaped nano silicon powder for lithium ion battery negative electrode, negative electrode material and preparation method |
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| WO2023125262A1 (en) * | 2021-12-27 | 2023-07-06 | 上海耀鸿科技股份有限公司 | Modified aluminum alloy and preparation method therefor |
| WO2023125263A1 (en) * | 2021-12-27 | 2023-07-06 | 上海耀鸿科技股份有限公司 | Composite rare earth alloy for aluminum alloy modification and preparation method therefor |
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