CN112853239A - Gradient structure and reinforced layer of surface of superfine crystal magnesium alloy plate and preparation method thereof - Google Patents

Gradient structure and reinforced layer of surface of superfine crystal magnesium alloy plate and preparation method thereof Download PDF

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CN112853239A
CN112853239A CN202011529185.7A CN202011529185A CN112853239A CN 112853239 A CN112853239 A CN 112853239A CN 202011529185 A CN202011529185 A CN 202011529185A CN 112853239 A CN112853239 A CN 112853239A
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magnesium alloy
strengthening layer
gradient structure
alloy plate
crystal magnesium
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CN112853239B (en
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王宗申
陈磊
朱立华
管延锦
于从潇
郑宏宇
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Shandong University
Shandong University of Technology
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    • 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
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21DWORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D31/00Other methods for working sheet metal, metal tubes, metal profiles
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0081Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets

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Abstract

The invention discloses a gradient tissue structure and a strengthening layer of the surface of an ultrafine crystal magnesium alloy plate and a preparation method thereof, comprising the following steps: and carrying out isothermal die pressing deformation treatment on the magnesium alloy plate subjected to annealing treatment to obtain an ultrafine-crystal magnesium alloy plate, and then carrying out ultrasonic shot blasting treatment on the ultrafine-crystal magnesium alloy plate to obtain a surface gradient structure and a strengthening layer. The isothermal die pressing deformation process and the ultrasonic shot blasting process are combined, so that the grain size of the AZ31 magnesium alloy can be further reduced compared with a single process, an ultrafine grain and surface gradient tissue structure and a strengthening layer are obtained, and the surface hardness of the material is enhanced. The AZ31 magnesium alloy without isothermal die pressing deformation and ultrasonic shot blasting treatment had an average grain size of 13.23 μm and a surface hardness of 60 HV. After the composite process is adopted, the grain size of the magnesium alloy is reduced by 43.16%, and the hardness is improved by 296.67%.

Description

Gradient structure and reinforced layer of surface of superfine crystal magnesium alloy plate and preparation method thereof
Technical Field
The invention belongs to the technical field of metal material modification, and relates to a gradient structure and a strengthening layer of the surface of an ultrafine crystal magnesium alloy plate and a preparation method thereof, in particular to a preparation method for obtaining the gradient structure and the strengthening layer of the surface of the ultrafine crystal magnesium alloy plate by using an isothermal die pressing deformation and ultrasonic shot blasting composite process.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Magnesium alloy is the lightest metal structural material at present, and the density of the magnesium alloy is only 1.8g/cm3And the composite material has excellent heat dissipation and shock absorption performance, and has wide application prospect in the industries of aviation, aerospace, transportation, biomedicine, electronics and the like. However, the magnesium alloy still has the problems of poor room temperature plastic deformation capability, large brittleness, low absolute strength, poor corrosion resistance and the like, and the application of the magnesium alloy is limited.
Die pressing deformation is a severe plastic deformation technique used for preparing ultra-fine grain metal plates. The plate sample is alternately bent and flattened to deform, so that a great amount of plastic strain can be accumulated in the material to refine crystal grains and obtain an ultrafine crystal structure under the condition of not changing the shape and the size of the sample.
In the prior art, the AZ31 magnesium alloy plate is subjected to 2-pass isothermal die pressing deformation in a previous test, the grain refining effect is obvious, and the average levels of the strength and the hardness of the plate are obviously improved. However, the surface grain structure of the AZ31 magnesium alloy sheet subjected to isothermal die pressing deformation is coarser than that of the magnesium alloy sheet subjected to isothermal die pressing deformation, and microcracks appear on the surface of the magnesium alloy sheet, so that the plasticity index of the sheet is reduced, and the surface hardness is not improved. Therefore, the superfine crystal magnesium alloy plate and the surface gradient structure and the strengthening layer thereof are difficult to obtain only by adopting an isothermal die pressing deformation mode.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a gradient structure and a strengthening layer on the surface of an ultrafine crystal magnesium alloy plate and a preparation method thereof. The preparation method has the advantages of grain refinement, hardness improvement, greenness, no pollution and the like, and has wide application prospect.
In order to solve the technical problems, the invention adopts the following technical scheme:
in a first aspect, the invention provides a method for preparing a gradient structure and a strengthening layer on the surface of an ultrafine crystal magnesium alloy plate, which comprises the following steps:
and (3) carrying out isothermal die pressing deformation treatment on the magnesium alloy plate subjected to annealing treatment, and then carrying out ultrasonic shot blasting treatment on the magnesium alloy plate to obtain the surface gradient structure and the strengthening layer of the superfine crystal magnesium alloy plate.
In a second aspect, the invention provides a gradient structure and a strengthening layer on the surface of an ultrafine crystal magnesium alloy plate, which are prepared by the preparation method.
Compared with the prior art, the beneficial effects of the above one or more embodiments of the invention are as follows:
(1) the preparation method provided by the invention is convenient and simple to operate, low in energy consumption, green and pollution-free.
(2) The invention combines the isothermal die pressing deformation process and the ultrasonic shot blasting process, can further reduce the grain size of the magnesium alloy plate compared with a single process, obtains a surface gradient structure and a strengthening layer, and improves the surface hardness of the material. The magnesium alloy which is not subjected to isothermal die pressing deformation and ultrasonic shot blasting treatment has an average grain size of 13.23 mu m and surface hardness of 60 HV. After the composite process is adopted, the average grain size of the magnesium alloy is reduced by 43.16%, and the surface hardness is improved by 296.67%.
(3) In the preparation method, the influence of the ultrasonic shot blasting technology on the surface texture and the hardness is more obvious.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic diagram of the process of isothermal die pressing deformation and ultrasonic shot peening according to an embodiment of the present invention.
FIG. 2 is a microstructure diagram obtained in example 1 and comparative examples 1 to 3, wherein (a) is the microstructure diagram of example 1, (b) is the microstructure diagram of comparative example 1, (c) is the microstructure diagram of comparative example 2, and (d) is the microstructure diagram of comparative example 3.
Fig. 3 is a hardness profile of the surface layer obtained in example 1 and comparative examples 1 to 3, wherein (a) is the hardness profile of example 1, (b) is the hardness profile of comparative example 1, (c) is the hardness profile of comparative example 2, and (d) is the hardness profile of comparative example 3.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In a first aspect, the invention provides a method for preparing a gradient structure and a strengthening layer on the surface of an ultrafine crystal magnesium alloy plate, which comprises the following steps:
and carrying out isothermal die pressing deformation treatment on the magnesium alloy plate subjected to annealing treatment to obtain an ultrafine-crystal magnesium alloy plate, and then carrying out ultrasonic shot blasting treatment on the ultrafine-crystal magnesium alloy plate to obtain a surface gradient structure and a strengthening layer.
In some embodiments, the temperature of the annealing treatment is 280-320 ℃, and the annealing time is 50-70 min.
In some embodiments, the magnesium alloy sheet is subjected to isothermal die pressing deformation at a pressing rate of 4.9-5.1mm/min and at a temperature of 199-.
Furthermore, the side surface inclination angle (theta) of the bending tooth subjected to isothermal die pressing deformation treatment is 40-50 degrees, and the top surface width (T) of the bending tooth is the same as the thickness of the magnesium alloy sheet.
In some embodiments, the steel balls have a grain size of 2.5 to 3.5mm in the ultrasonic peening treatment.
Furthermore, the hardness of the steel ball is 45-55 HRC.
Further, the steel balls are paved at the bottom of the shot blasting chamber.
Furthermore, the working amplitude of the experimental device for ultrasonic shot blasting is 35-45 μm, and the working time is 80-120 s.
Further, the working amplitude of the ultrasonic shot-peening experimental apparatus was 40 μm and the working time was 100 seconds.
In a second aspect, the invention provides a gradient structure and a strengthening layer on the surface of an ultrafine crystal magnesium alloy plate, which are prepared by the preparation method.
Example 1
1) And (3) annealing the commercial AZ31 magnesium alloy rolled plate with the thickness of 2mm at the temperature of 300 ℃ for 60 min.
2) On a YAW-5000F type microcomputer control electro-hydraulic servo pressure tester, isothermal die pressing deformation of 2 times is carried out on the magnesium alloy plate, the pressing rate of the die pressing experiment is 5mm/min, and the temperature is 200 ℃.
3) Putting cast steel shots with the diameter of 3mm and the hardness of 45-55HRC into a shot blasting chamber, wherein the number of the steel balls is just paved at the bottom of the shot blasting chamber, then fixing the magnesium alloy plate (with the size of 25mm multiplied by 2mm) after die pressing deformation on the upper surface of a workpiece fixing device, setting the distance between an ultrasonic tool head and a sample to be 7.5mm, setting the working amplitude of an ultrasonic shot blasting experimental device to be 40 mu m, and setting the working time to be 100 s.
4) And starting the ultrasonic generator, converting the power frequency alternating current into an electric signal by the ultrasonic generator, and transmitting the electric signal to the ultrasonic transducer.
5) The ultrasonic transducer converts the electric signal into ultrasonic vibration which is transmitted to the ultrasonic tool head through the ultrasonic amplitude transformer to generate mechanical vibration of 40 mu m.
6) The cast steel shot in the shot blasting chamber is driven by the vibrating ultrasonic tool head to impact the surface of the magnesium alloy plate, after one-time impact is finished, the shot falls back to the tool head again under the action of rebound and gravity, is driven by the tool head to impact a sample again, and is repeatedly carried out for many times until the set impact time is reached.
Example 2
1) And (3) annealing the commercial AZ31 magnesium alloy rolled plate with the thickness of 2mm at 290 ℃ for 65 min.
2) On a YAW-5000F type microcomputer control electro-hydraulic servo pressure tester, isothermal die pressing deformation of 2 times is carried out on the magnesium alloy plate, the pressing rate of the die pressing experiment is 5.1mm/min, and the temperature is 201 ℃.
3) Putting cast steel shots with the diameter of 3mm and the hardness of 45-55HRC into a shot blasting chamber, wherein the number of the steel balls is just paved at the bottom of the shot blasting chamber, then fixing the magnesium alloy plate (with the size of 25mm multiplied by 2mm) after die pressing deformation on the upper surface of a workpiece fixing device, setting the distance between an ultrasonic tool head and a sample to be 7.5mm, setting the working amplitude of an ultrasonic shot blasting experimental device to be 42 mu m, and setting the working time to be 90 s.
4) And starting the ultrasonic generator, converting the power frequency alternating current into an electric signal by the ultrasonic generator, and transmitting the electric signal to the ultrasonic transducer.
5) The ultrasonic transducer converts the electric signal into ultrasonic vibration which is transmitted to the ultrasonic tool head through the ultrasonic amplitude transformer to generate mechanical vibration of 40 mu m.
6) The cast steel shot in the shot blasting chamber is driven by the vibrating ultrasonic tool head to impact the surface of the magnesium alloy plate, after one-time impact is finished, the shot falls back to the tool head again under the action of rebound and gravity, is driven by the tool head to impact a sample again, and is repeatedly carried out for many times until the set impact time is reached.
Example 3
1) And (3) annealing the commercial AZ31 magnesium alloy rolled plate with the thickness of 2mm at 290 ℃ for 55 min.
2) On a YAW-5000F type microcomputer control electro-hydraulic servo pressure tester, isothermal die pressing deformation of 2 times is carried out on the magnesium alloy plate, the pressing rate of the die pressing experiment is 4.9mm/min, and the temperature is 200 ℃.
3) Putting cast steel shots with the diameter of 3mm and the hardness of 45-55HRC into a shot blasting chamber, wherein the number of the steel balls is just paved at the bottom of the shot blasting chamber, then fixing the magnesium alloy plate (with the size of 25mm multiplied by 2mm) after die pressing deformation on the upper surface of a workpiece fixing device, setting the distance between an ultrasonic tool head and a sample to be 7.5mm, setting the working amplitude of an ultrasonic shot blasting experimental device to be 40 mu m, and setting the working time to be 100 s.
4) And starting the ultrasonic generator, converting the power frequency alternating current into an electric signal by the ultrasonic generator, and transmitting the electric signal to the ultrasonic transducer.
5) The ultrasonic transducer converts the electric signal into ultrasonic vibration which is transmitted to the ultrasonic tool head through the ultrasonic amplitude transformer to generate mechanical vibration of 40 mu m.
6) The cast steel shot in the shot blasting chamber is driven by the vibrating ultrasonic tool head to impact the surface of the magnesium alloy plate, after one-time impact is finished, the shot falls back to the tool head again under the action of rebound and gravity, is driven by the tool head to impact a sample again, and is repeatedly carried out for many times until the set impact time is reached.
Comparative example 1
1) And (3) annealing the commercial AZ31 magnesium alloy rolled plate with the thickness of 2mm at the temperature of 300 ℃ for 60 min.
2) On a YAW-5000F type microcomputer control electro-hydraulic servo pressure tester, isothermal die pressing deformation of 2 times is carried out on the magnesium alloy plate, the pressing rate of the die pressing experiment is 5mm/min, and the temperature is 200 ℃.
Comparative example 2
1) And (3) annealing the commercial AZ31 magnesium alloy rolled plate with the thickness of 2mm at the temperature of 300 ℃ for 60 min.
2) Putting cast steel shots with the diameter of 3mm and the hardness of 45-55HRC into a shot blasting chamber, wherein the number of the steel balls is just paved at the bottom of the shot blasting chamber, fixing a magnesium alloy plate (with the size of 25mm multiplied by 2mm) subjected to isothermal die pressing deformation on the upper surface of a workpiece fixing device, setting the distance between an ultrasonic tool head and a sample to be 7.5mm, setting the working amplitude of an ultrasonic shot blasting experimental device to be 40 mu m, and setting the working time to be 100 s.
3) And starting the ultrasonic generator, converting the power frequency alternating current into an electric signal by the ultrasonic generator, and transmitting the electric signal to the ultrasonic transducer.
4) The ultrasonic transducer converts the electric signal into ultrasonic vibration which is transmitted to the ultrasonic tool head through the ultrasonic amplitude transformer to generate mechanical vibration of 40 mu m.
5) The cast steel shot in the shot blasting chamber is driven by the vibrating ultrasonic tool head to impact the surface of the magnesium alloy plate, after one-time impact is finished, the shot falls back to the tool head again under the action of rebound and gravity, is driven by the tool head to impact a sample again, and is repeatedly carried out for many times until the set impact time is reached.
Comparative example 3
Without the initial conditions of isothermal die pressing deformation and ultrasonic shot blasting.
Table 1 results of performance testing
Figure BDA0002851585110000071
FIG. 2 is a microstructure diagram of example 1 and comparative examples 1 to 3 after treatment. As can be seen from fig. 2, comparative example 3, which was not subjected to any treatment, had the largest average grain size; comparative example 1, which was subjected to isothermal die pressing deformation only, obtained only an ultrafine grained microstructure; compared with the comparative example 1, the comparative example 2 which only undergoes the ultrasonic shot blasting process has more obvious effect of grain refinement, can obtain a surface gradient structure, but still has a coarse grain structure inside the plate; and the average grain size of the example 1 which is subjected to the isothermal die pressing deformation and ultrasonic shot blasting composite process is the smallest, so that the superfine crystal magnesium alloy plate with the surface gradient structure can be obtained.
Fig. 3 is a surface hardness distribution curve of example 1 and comparative examples 1 to 3 after treatment. As can be seen from fig. 3, neither comparative example 3 without any treatment nor comparative example 1 subjected to isothermal press-deformation alone obtained a surface reinforcing layer; comparative example 2, which was subjected to only the ultrasonic shot peening process, could obtain a surface strengthened layer, but the difference between the surface hardness and the interior was large; in example 1, which is subjected to the isothermal die pressing deformation and ultrasonic shot peening combined process, a surface strengthening layer can be obtained, and the internal hardness level is high.
Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive faculty, based on the technical solutions of the present invention.

Claims (10)

1. A method for preparing a gradient structure and a strengthening layer on the surface of an ultrafine crystal magnesium alloy plate is characterized by comprising the following steps: the method comprises the following steps:
and carrying out isothermal die pressing deformation treatment on the magnesium alloy plate subjected to annealing treatment to obtain an ultrafine-crystal magnesium alloy plate, and then carrying out ultrasonic shot blasting treatment on the ultrafine-crystal magnesium alloy plate to obtain a surface gradient structure and a strengthening layer.
2. The method for preparing the superfine crystal magnesium alloy surface gradient structure and the strengthening layer according to claim 1, which is characterized in that: the temperature of the annealing treatment is 280-320 ℃, and the annealing time is 50-70 min.
3. The method for preparing the superfine crystal magnesium alloy surface gradient structure and the strengthening layer according to claim 1, which is characterized in that: the pressing rate of the magnesium alloy plate subjected to isothermal die pressing deformation treatment is 4.9-5.1mm/min, and the temperature is 199-.
4. The method for preparing the superfine crystal magnesium alloy surface gradient structure and the strengthening layer according to claim 3, which is characterized in that: the side surface inclination angle of the bending tooth subjected to isothermal die pressing deformation treatment is 40-50 degrees, and the width of the top surface of the bending tooth is the same as the thickness of the magnesium alloy sheet.
5. The method for preparing the superfine crystal magnesium alloy surface gradient structure and the strengthening layer according to claim 1, which is characterized in that: in the ultrasonic shot blasting treatment, the grain diameter of the steel ball is 2.5-3.5 mm.
6. The method for preparing the superfine crystal magnesium alloy surface gradient structure and the strengthening layer according to claim 5, which is characterized in that: the hardness of the steel ball is 45-55 HRC.
7. The method for preparing the superfine crystal magnesium alloy surface gradient structure and the strengthening layer according to claim 5, which is characterized in that: the steel balls are spread on the bottom of the shot blasting chamber.
8. The method for preparing the superfine crystal magnesium alloy surface gradient structure and the strengthening layer according to claim 5, which is characterized in that: the working amplitude of the experimental device for ultrasonic shot blasting is 35-45 mu m, and the working time is 80-120 s.
9. The method for preparing the superfine crystal magnesium alloy surface gradient structure and the strengthening layer according to claim 8, wherein the method comprises the following steps: the working amplitude of the experimental device for ultrasonic shot blasting is 40 mu m, and the working time is 100 s.
10. A gradient structure and a strengthening layer of the surface of an ultrafine crystal magnesium alloy plate are characterized in that: prepared by the preparation method of any one of claims 1 to 9.
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