CN115216675B - Method for preparing superfine layered twin crystal structure on surface of aluminum alloy - Google Patents

Method for preparing superfine layered twin crystal structure on surface of aluminum alloy Download PDF

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CN115216675B
CN115216675B CN202210895226.7A CN202210895226A CN115216675B CN 115216675 B CN115216675 B CN 115216675B CN 202210895226 A CN202210895226 A CN 202210895226A CN 115216675 B CN115216675 B CN 115216675B
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twin
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aluminum alloy
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CN115216675A (en
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赵庆龙
刘帅
刘肖
姜启川
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Jilin University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/12Alloys based on aluminium with copper as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F3/00Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention belongs to the technical field of metal material processing, and particularly relates to a method for preparing a superfine layered twin crystal structure on the surface of an aluminum alloy, which comprises the following steps of 1: preparing an Al-Cu alloy melt, preparing materials according to the content of each alloy component, placing the materials in a smelting furnace to obtain a molten Al-Cu alloy, and then preserving heat for 10-20min; step 2: adding twin crystal TiC particles, adding the twin crystal TiC particles into the molten Al-Cu alloy obtained in the step (1), mechanically stirring for 2-3min, then carrying out ultrasonic treatment, and pouring and forming; and step 3: the method comprises the steps of remelting on the surface of the laser, polishing the surface of the Al-Cu alloy plate by using sand paper, cleaning the surface of the Al-Cu alloy plate by using an organic solvent, and then carrying out laser remelting treatment on the surface of the alloy at room temperature to obtain a twin crystal layer on the surface of the aluminum alloy.

Description

Method for preparing superfine layered twin crystal structure on surface of aluminum alloy
Technical Field
The invention relates to the technical field of metal material processing, in particular to a method for preparing a superfine layered twin crystal structure on the surface of an aluminum alloy.
Background
The current research shows that the twin crystal structure is introduced into the alloy, so that the strength of the material can be improved, the plasticity of the material can be improved, and the toughening of the metal material can be realized (Science, 2009, 324, 349 pages). For example, for metals such as Nickel and copper, an ultra-fine twin Structure has been successfully prepared on the surface by a surface mechanical grinding method, and the thickness of a single layer of twin is below 10 μm, even reaching the nanometer level (train-Induced ultra and ultra-stable nano-structured in Nickel, science,2013, volume 342, page 337). This can significantly increase the hardness and strength of the metal.
Nevertheless, it is difficult to produce ultra-fine twin crystals on the surface of the aluminum alloy at present because the aluminum alloy has high energy of stacking faults and it is difficult to form a lamellar twin structure by mechanical grinding, plastic deformation, or the like. Although feathered twin crystals are occasionally formed inside a semicontinuous-cast aluminum alloy, twin-boundary intervals are several tens of micrometers, and are not formed on the surface. The laser remelting technology is to utilize high-energy laser particle beams emitted by a laser to perform selective melting on the surface of a material to be processed without element addition. Laser remelting forms a molten pool quickly in a surface selection area, and the solidification speed is high. Therefore, laser remelting can significantly refine grains, but there is no method for preparing a twin structure by laser processing an aluminum alloy. At present, a surface treatment method is lacked, and an ultra-fine twin crystal structure can be prepared on the surface of the aluminum alloy to provide the surface performance of the aluminum alloy.
Based on the above, we propose a method for preparing an ultrafine layered twin structure on the surface of an aluminum alloy.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the problems occurring in the prior art.
Therefore, the invention aims to provide a method for preparing a superfine layered twin crystal structure on the surface of an aluminum alloy, the method has simple process and easy operation, and the obtained twin crystal structure is greatly beneficial to improving the surface characteristics and the mechanical properties of the aluminum alloy.
In order to solve the above technical problems, according to one aspect of the present invention, the present invention provides the following technical solutions:
a method for preparing an ultrafine layered twin crystal structure on the surface of an aluminum alloy comprises the following steps:
step 1: preparation of Al-Cu alloy melt
Preparing materials according to the component content of each alloy, placing the materials in a smelting furnace to obtain molten Al-Cu alloy, and then preserving heat for 10-20min;
step 2: adding twin crystal TiC particles
Adding twin crystal TiC particles into the molten Al-Cu alloy obtained in the step (1), mechanically stirring for 2-3min, then carrying out ultrasonic treatment, and pouring and forming, wherein the twin crystal TiC particles are nearly spherical and have the size of 60-200nm;
adjusting the temperature of the melt to 720 ℃, standing and preserving heat for 3-5min, then adding a slag removing agent into the alloy melt, stirring for 1-2min, then slagging, then pouring the melt into a steel mold, and cooling to room temperature to obtain an Al-Cu alloy plate containing twin crystal TiC particles;
and step 3: laser surface remelting
And (2) polishing the surface of the Al-Cu alloy plate by using sand paper, cleaning the surface of the Al-Cu alloy plate by using an organic solvent, and then carrying out laser remelting treatment on the surface of the Al-Cu alloy plate at room temperature to obtain a twin crystal layer on the surface of the Al alloy.
As a preferred scheme of the method for preparing the superfine layered twin crystal structure on the surface of the aluminum alloy, the method comprises the following steps: the mass fraction of the added TiC particles is 0.1-2%, and the mass fraction of the Cu element is 2-20%.
As a preferred scheme of the method for preparing the superfine layered twin crystal structure on the surface of the aluminum alloy, the method comprises the following steps: in the step 3, the diameter of a laser spot is 1-3mm, the laser power is 1-3kW, and the scanning speed is 1-30mm/min.
As a preferred scheme of the method for preparing the superfine layered twin crystal structure on the surface of the aluminum alloy, the method comprises the following steps: the prepared surface twin layer is characterized in that: the twin boundary spacing is below 10 microns, and the twin structure length is above 10 mm.
As a preferable scheme of the method for preparing the superfine layered twin crystal structure on the surface of the aluminum alloy, the method comprises the following steps: the TiC contains a twin structure, can be replaced by other nucleation particles containing the twin structure, and is one of carbide, boride and oxide containing the twin structure.
As a preferred scheme of the method for preparing the superfine layered twin crystal structure on the surface of the aluminum alloy, the method comprises the following steps: the method can also be applied to the preparation of surface twin crystal structures of Al-Mg, al-Zn binary alloys and Al-Zn-Mg, al-Cu-Mg multi-element alloys.
As a preferable scheme of the method for preparing the superfine layered twin crystal structure on the surface of the aluminum alloy, the method comprises the following steps: the preparation method of the twin crystal TiC particles comprises the following steps: weighing aluminum powder, titanium powder and carbon powder according to the mass ratio of aluminum to titanium to carbon being equal to 70:24:6 for later use; aluminum powder, titanium powder and carbon powder are mixed by ball milling to prepare a pressed compact; and sintering the pressed compact in a protective atmosphere at the sintering temperature of 800-900 ℃.
Compared with the prior art, the invention has the beneficial effects that: the process is simple, the operation is easy, and the obtained twin crystal structure is beneficial to improving the surface characteristics and the mechanical properties of the aluminum alloy.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and detailed embodiments, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without inventive labor. Wherein:
FIG. 1 is a metallographic photograph taken at 50 times the surface of a sample according to comparative example 1 of the present invention after laser remelting treatment;
FIG. 2 is a metallographic photograph taken at 50 times the surface of a sample after laser remelting treatment in example 1 of the present invention;
FIG. 3 is an EBSD photograph of twin structure of the test piece after the laser remelting treatment in example 1 of the present invention.
FIG. 4 is a polar view of the twin orientation relationship of the region of FIG. 3;
FIG. 5 is a flow chart of the steps of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described herein, and it will be apparent to those of ordinary skill in the art that the present invention may be practiced without departing from the spirit and scope of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Next, the present invention will be described in detail with reference to the drawings, wherein for convenience of illustration, the cross-sectional view of the device structure is not enlarged partially according to the general scale, and the drawings are only examples, which should not limit the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Comparative example 1
The Al-Cu alloy plate is not added with TiC particles, and the mass fraction of the Al-Cu alloy copper is 10 +/-0.5%.
The preparation method comprises the following steps:
step 1: preparation of Al-Cu alloy melt
Preparing materials according to the content of each alloy component, placing the materials into a smelting furnace, heating the smelting furnace to 800 +/-10 ℃, smelting for 2 hours to ensure that molten Al-Cu alloy is obtained, and then preserving heat for 15min;
adjusting the temperature of the melt to 720 ℃, standing and preserving heat for 5min, then adding a slag removing agent into the alloy melt, stirring for 2min, then slagging, then pouring the melt into a steel mold, and cooling to room temperature to obtain an Al-Cu alloy plate;
and 2, step: laser surface remelting
And (2) polishing the surface of the Al-Cu alloy plate by using sand paper, cleaning the surface of the Al-Cu alloy plate by using an organic solvent, then carrying out laser remelting treatment on the surface of the alloy at room temperature to obtain a growth twin crystal layer on the surface of the aluminum alloy, wherein the laser wavelength is 1070nm, the spot diameter is 2.5mm, the laser power is 1500W, and the scanning speed is 10mm/min.
The metallographic photograph of the surface of the sample after the laser remelting treatment is shown in fig. 1, after the laser remelting treatment, a growth twin structure does not appear in an Al-Cu alloy molten pool without TiC particles, the bottom of the molten pool shows that the grains are still relatively coarse and grow epitaxially along a matrix structure, but secondary dendrite arms are significantly refined.
Example 1
And the Al-Cu alloy plate added with TiC particles comprises 5% of Al-Cu alloy copper by mass.
The preparation method comprises the following steps:
step 1: preparation of Al-Cu alloy melt
Preparing materials according to the content of each alloy component, placing the materials into a smelting furnace, heating the smelting furnace to 800 +/-10 ℃, smelting for 2 hours to ensure that molten Al-Cu alloy is obtained, and then preserving heat for 15min;
and 2, step: adding twin crystal TiC particles
Adding twin crystal TiC particles into the molten Al-Cu alloy obtained in the step (1), mechanically stirring for 2min, and then carrying out ultrasonic treatment, wherein the addition amount of the TiC particles is 0.5%, the twin crystal TiC particles are nearly spherical, and the size of the twin crystal TiC particles is 60-200nm;
adjusting the temperature of the melt to 720 ℃, standing and preserving heat for 5min, then adding a slag removing agent into the alloy melt, stirring for 2min, then slagging, then pouring the melt into a steel mold, and cooling to room temperature to obtain an Al-Cu alloy plate containing twin crystal TiC particles;
and step 3: laser surface remelting
And (2) polishing the surface of the Al-Cu alloy plate by using sand paper, cleaning the surface of the Al-Cu alloy plate by using an organic solvent, then carrying out laser remelting treatment on the surface of the alloy at room temperature to obtain a growth twin crystal layer on the surface of the aluminum alloy, wherein the laser wavelength is 1070nm, the spot diameter is 2.5mm, the laser power is 1500W, and the scanning speed is 10mm/min.
The metallographic photograph of the surface of the Al-Cu sample containing the TiC particles after the laser remelting treatment is shown in figure 2, after the laser remelting treatment, an obvious twin structure appears in an Al-Cu alloy molten pool added with the TiC particles, and the whole width of the twin structure is 200-300 mu m. The twin appearance mainly takes cluster-shaped twin as a main part and is accompanied by a small amount of isolated twin. The densely arranged cluster type twin dendritic crystal has a finer structure, the main direction of the dendritic crystal is consistent with the temperature gradient direction, and the arrangement of the twin crystal lamina is compact and ordered. The EBSD is used for carrying out high power analysis on the part, as shown in figure 3, the width of a single twin crystal is 2-5 mu m, and the characteristic that coherent twin boundaries and non-coherent twin boundaries are alternately arranged is shown. The polar diagram (FIG. 4) confirms that the {111} crystal plane is the twin plane.
Example 2
And the Al-Cu alloy plate added with TiC particles comprises 20% of Al-Cu alloy copper by mass.
The preparation method comprises the following steps:
step 1: preparation of Al-Cu alloy melt
Preparing materials according to the component content of each alloy, placing the materials into a smelting furnace, heating the smelting furnace to 800 +/-10 ℃, smelting for 2 hours to ensure that molten Al-Cu alloy is obtained, and then preserving heat for 15min:
step 2: adding twin crystal TiC particles
Adding twin crystal TiC particles into the molten Al-Cu alloy obtained in the step (1), mechanically stirring for 2min, and then carrying out ultrasonic treatment, wherein the addition amount of the TiC particles is 0.1%, the TiC particles are nearly spherical and have the size of 60-200nm;
adjusting the temperature of the melt to 720 ℃, standing and preserving heat for 5min, then adding a slag removing agent into the alloy melt, stirring for 2min, then slagging, then pouring the melt into a steel mold, and cooling to room temperature to obtain an Al-Cu alloy plate containing twin crystal TiC particles;
and step 3: laser surface remelting
The method comprises the following steps of polishing the surface of an Al-Cu alloy plate by using abrasive paper, cleaning the surface of the Al-Cu alloy plate by using an organic solvent, and then carrying out laser remelting treatment on the surface of the Al-Cu alloy plate at room temperature to obtain a twin crystal layer on the surface of the Al alloy plate, wherein the laser wavelength is 1070nm, the spot diameter is 2.5mm, the laser power is 1500W, and the scanning speed is 10mm/min.
The Al-Cu sample containing the twin crystal TiC particles forms a large number of twin crystal tissues in a molten pool after laser remelting treatment, and the width of a single twin crystal is less than 10 mu m.
Comparative example 2
An Al-Cu alloy plate added with 2.5 percent of TiC particles, wherein the mass fraction of the copper content of the Al-Cu alloy is 10 +/-0.5 percent.
The preparation method comprises the following steps:
step 1: preparation of Al-Cu alloy melt
Preparing materials according to the content of each alloy component, placing the materials into a smelting furnace, heating the smelting furnace to 800 +/-10 ℃, smelting for 2 hours to ensure that molten Al-Cu alloy is obtained, and then preserving heat for 15min;
adjusting the temperature of the melt to 720 ℃, standing and preserving heat for 5min, then adding a slag removing agent into the alloy melt, stirring for 2min, then slagging, then pouring the melt into a steel mold, and cooling to room temperature to obtain an Al-Cu alloy plate;
step 2: adding twin crystal TiC particles
Adding twin crystal TiC particles into the molten Al-Cu alloy obtained in the step (1), mechanically stirring for 2min, and then carrying out ultrasonic treatment, wherein the addition amount of the TiC particles is 2.5%, the TiC particles are nearly spherical and have the size of 60-200nm;
adjusting the temperature of the melt to 720 ℃, standing and preserving heat for 5min, then adding a slag removing agent into the alloy melt, stirring for 2min, then slagging, then pouring the melt into a steel mold, and cooling to room temperature to obtain an Al-Cu alloy plate containing twin crystal TiC particles;
and step 3: laser surface remelting
And (2) polishing the surface of the Al-Cu alloy plate by using sand paper, cleaning the surface of the Al-Cu alloy plate by using an organic solvent, then carrying out laser remelting treatment on the surface of the alloy at room temperature to obtain a growth twin crystal layer on the surface of the aluminum alloy, wherein the laser wavelength is 1070nm, the spot diameter is 2.5mm, the laser power is 1500W, and the scanning speed is 10mm/min.
An Al-Cu alloy plate to which 2.5% by mass of TiC particles are added exhibits a fine equiaxed grain structure; the sample is still equiaxial grains after laser remelting treatment, and a twin structure does not appear.
While the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the disclosed embodiments of the invention may be used in any combination, provided that no structural conflict exists, and the combinations are not exhaustively described in this specification merely for the sake of brevity and resource conservation. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (5)

1. A method for preparing an ultrafine layered twin crystal structure on the surface of an aluminum alloy is characterized by comprising the following steps: the method comprises the following steps:
step 1: preparation of Al-Cu alloy melt
Preparing materials according to the component content of each alloy, placing the materials in a smelting furnace to obtain molten Al-Cu alloy, and then preserving heat for 10-20min;
step 2: adding twin crystal TiC particles
Adding twin crystal TiC particles into the molten Al-Cu alloy obtained in the step (1), mechanically stirring for 2-3min, then carrying out ultrasonic treatment, and pouring and forming, wherein the twin crystal TiC particles are nearly spherical and have the size of 60-200nm;
adjusting the temperature of the melt to 720 ℃, standing and preserving heat for 3-5min, then adding a slag removing agent into the alloy melt, stirring for 1-2min, then slagging, then pouring the melt into a steel mold, and cooling to room temperature to obtain an Al-Cu alloy plate containing twin crystal TiC particles;
the mass fraction of the added TiC particles is 0.1-2%, and the mass fraction of the Cu element is 2-20%;
and step 3: laser surface remelting
And (3) polishing the surface of the Al-Cu alloy plate by using sand paper, cleaning the surface of the Al-Cu alloy plate by using an organic solvent, then carrying out laser remelting treatment on the surface of the alloy at room temperature to obtain a growing twin crystal layer on the surface of the aluminum alloy, wherein in the step 3, the diameter of a laser spot is 1-3mm, the laser power is 1-3kW, and the scanning speed is 1-30mm/min.
2. The method for preparing the superfine layered twin structure on the surface of the aluminum alloy according to claim 1, which is characterized in that: the prepared surface twin layer is characterized in that: the twin boundary spacing is below 10 microns, and the twin structure length is above 10 mm.
3. The method for preparing the superfine layered twin structure on the surface of the aluminum alloy according to claim 1, which is characterized in that: the TiC contains a twin structure, can be replaced by other nucleation particles containing the twin structure, and is one of carbide, boride and oxide containing the twin structure.
4. The method for preparing the superfine layered twin structure on the surface of the aluminum alloy according to any one of claims 1 to 3, wherein the method comprises the following steps: the method can also be applied to preparing surface twin crystal structures from Al-Mg, al-Zn binary alloys and Al-Zn-Mg, al-Cu-Mg multi-element alloys.
5. The method for preparing the superfine layered twin structure on the surface of the aluminum alloy according to claim 1, which is characterized in that: the preparation method of the twin crystal TiC particles comprises the following steps: according to the aluminum: titanium: the mass ratio of carbon is equal to 70:24: weighing aluminum powder, titanium powder and carbon powder for later use; aluminum powder, titanium powder and carbon powder are mixed by ball milling to prepare a pressed compact; and sintering the pressed compact in a protective atmosphere at the sintering temperature of 800-900 ℃.
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