CN112663008B - Method for preparing magnesium-aluminum composite board by utilizing radio frequency magnetic control - Google Patents
Method for preparing magnesium-aluminum composite board by utilizing radio frequency magnetic control Download PDFInfo
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Abstract
The invention belongs to the technical field of light alloy, and particularly relates to a method for preparing a magnesium-aluminum composite plate by utilizing radio frequency magnetic control, which comprises the following steps: (1) preparing a matrix: putting the cleaned magnesium alloy matrix into a sample sending chamber of radio frequency magnetron sputtering equipment for vacuumizing; (2) pre-sputtering: respectively carrying out pre-sputtering on the magnesium target and the aluminum target in the sputtering cavity; (3) sample feeding: conveying the magnesium alloy matrix to a sample table in a sputtering cavity; (4) washing the cavity: opening an air inlet valve of the sputtering cavity, and adjusting the flow of the high-purity argon and the cleaning time; (5) heating the matrix: heating the magnesium alloy matrix, and then adjusting a sample rotating platform to rotate continuously; (6) sputtering: respectively carrying out radio frequency magnetron sputtering on the magnesium target material and the aluminum target material; (7) cold rolling: and performing cold rolling treatment on the single side sputtered with the aluminum to obtain the magnesium-aluminum composite plate. The magnesium-aluminum composite board prepared by the method has excellent comprehensive performance, realizes complete metallurgical bonding of the layer interface between magnesium and aluminum, and has high bonding strength.
Description
Technical Field
The invention belongs to the technical field of light alloys, and particularly relates to a method for preparing a magnesium-aluminum composite board by utilizing radio frequency magnetic control.
Background
Poor corrosion resistance of magnesium and magnesium alloys is one of the main reasons limiting their widespread use. In contrast, aluminum and aluminum alloys generally have excellent corrosion resistance and plastic formability, and have good surface repairability and decorativeness. Therefore, the laminated composite material formed by covering a layer of metal aluminum with good corrosion resistance on the surface of the magnesium alloy can protect the magnesium alloy and simultaneously can exert the advantages of high specific strength and specific rigidity, good damping performance, good electromagnetic wave shielding performance and the like of the magnesium alloy. It is expected that such magnesium-aluminum composite panels will be widely used in the aerospace, automotive and electronic industries to produce various thin-walled parts by stamping in the near future. The reported techniques for making magnesium aluminum composite panels are: the technology comprises the steps of vacuum diffusion welding, contact reaction brazing, hot pressing, explosion cladding, cold rolling, hot rolling, casting rolling and accumulative overlaying welding, and the technologies have higher interface bonding strength, but the layer interface is difficult to realize complete metallurgical bonding, so that the application of the magnesium-aluminum composite plate is limited.
The present invention is proposed to solve the above-mentioned technical problems.
Disclosure of Invention
In order to solve the defect that the interface of the middle layer of the magnesium-aluminum composite plate in the prior art is difficult to realize complete metallurgy, the invention aims to provide the method for preparing the magnesium-aluminum composite plate by using the radio frequency magnetic control.
The invention is realized by the following technical scheme:
a method for preparing a magnesium-aluminum composite plate by utilizing radio frequency magnetic control specifically comprises the following steps:
(1) Preparing a matrix: fixing the cleaned magnesium alloy substrate on a baffle, putting the magnesium alloy substrate into a sample conveying chamber of radio frequency magnetron sputtering equipment for vacuumizing, and then closing a vacuum pump of the sample conveying chamber;
(2) Pre-sputtering: respectively carrying out pre-sputtering on the magnesium target and the aluminum target in the sputtering cavity;
(3) Sample feeding: opening a gate between the sample conveying chamber and the sputtering cavity, and conveying the magnesium alloy matrix prepared in the step (1) to a sample table in the sputtering cavity;
(4) Washing a cavity: opening an air inlet valve of the sputtering cavity, and adjusting the flow of the high-purity argon and the cleaning time to clean the cavity;
(5) Heating the matrix: turning on a heater to heat the magnesium alloy substrate, and then adjusting the sample rotating platform to rotate continuously;
(6) Sputtering: after the heating of the substrate in the step (5) is finished, respectively setting the sputtering voltage, the working pressure, the sputtering time and the high-purity argon flow of the magnesium target and the aluminum target, and automatically executing the sputtering sequence set by the program: firstly sputtering the magnesium target material and introducing high-purity argon, closing the baffle plate after the magnesium target material sputtering is finished, then opening the baffle plate of the aluminum target material to start sputtering and introducing high-purity argon;
(7) Cold rolling: and after the sputtering is finished, cooling the cavity, taking out the sample, and then performing cold rolling treatment on the single surface sputtered with aluminum to obtain the magnesium-aluminum composite board.
The aluminum-magnesium composite plate is better in surface quality by performing cold rolling treatment on the single surface sputtered with aluminum, prevents surface oxidation, and solves the problems of easy surface oxidation and poor finish caused by hot rolling in the prior art.
Preferably, the step (1) of cleaning the magnesium alloy substrate specifically comprises: soaking the magnesium alloy substrate subjected to linear cutting in an acetic acid solution to remove surface oil stains, then ultrasonically cleaning the magnesium alloy substrate with deionized water for three times to perform single-side polishing, and respectively placing the magnesium alloy substrate after polishing in acetone, ethanol and deionized water to perform ultrasonic cleaning in sequence.
Preferably, the size of the magnesium alloy substrate after linear cutting is phi 76.2 multiplied by 5mm, the mass concentration of the acetic acid solution is 20-50 wt%, the soaking time in the acetic acid solution is 10-24h, the ultrasonic cleaning time of deionized water before polishing is 15-30 min/time, and the ultrasonic frequency is 100Hz;
and after polishing to a mirror surface, ultrasonically cleaning the mirror surface by using acetone, ethanol and deionized water for 15-30min at the ultrasonic frequency of 100Hz.
Preferably, the vacuum degree of the vacuum pumping in the step (1) is higher than 5X 10 -3 Torr。
Preferably, in the step (2), the magnesium target is pure magnesium with the purity of 99.99%, the aluminum target is pure aluminum with the purity of 99.9%, and the vacuum degree in the sputtering cavity during pre-sputtering is higher than 210 -7 The Torr, the voltage is 50-150V, the flow of high-purity argon is 20-40 sccm, the working pressure is 3-10 mTorr, the sputtering time is 20-30 min, and the temperature of the cavity is cooled to 20-30 ℃ after the sputtering is finished.
Preferably, the flow rate of the high-purity argon gas in the step (4) is 100sccm, and the cleaning time is 20-30 min.
Preferably, in the step (5), the magnesium alloy substrate is heated to 100-300 ℃, the rotating speed of the rotating platform is kept at 100rpm, the magnesium alloy is heated, and the phenomenon that a very thin amorphous layer is formed on the surface of the substrate firstly due to the low diffusion capacity of magnesium atoms and aluminum atoms in the process of undercooling and sputtering the magnesium and the aluminum on the substrate, so that the bonding degree with the substrate is reduced; another purpose of heating is to make the formed magnesium-aluminum composite plate uniform in structure and avoid the occurrence of a multilayer structure.
Preferably, the vacuum degree of the cavity during sputtering of the magnesium target in the step (6) is more than or equal to 2 × 10 -7 Torr, voltage is 50-100V, the flow of high-purity argon is kept at 20sccm, working pressure is 3mTorr, sputtering time is 30-60 min, and deposition distance is 10cm;
the vacuum degree of the cavity is more than or equal to 2 multiplied by 10 when the aluminum target material is sputtered -7 The Torr, the voltage is 100-200V, the flow of high-purity argon gas is kept at 20sccm, the working pressure is 3mTorr, the sputtering time is 3-6 h, and the deposition distance is 10cm;
in the step (6), the thickness of the magnesium layer sputtered by the magnesium target material is 1-3mm, and the thickness of the aluminum layer sputtered by the aluminum target material is 0.5-2mm.
Preferably, in the step (7), the cavity is cooled to 20-30 ℃ and the sample is taken out, and in the cold rolling treatment, the coating surface sputtered with aluminum faces upwards, and single-side cold rolling treatment is carried out, wherein the pressing amount is 1-2 mm.
Preferably, the magnesium alloy substrate in step (3) is kept stationary on the sample stage.
Compared with the prior art, the invention has the beneficial effects that:
(1) The magnesium-aluminum composite plate is obtained by sequentially sputtering and compounding the magnesium coating and the aluminum coating on the magnesium alloy substrate by utilizing a radio frequency magnetron sputtering technology and finally performing cold rolling treatment on the single surface sputtered with aluminum. The method is simple and easy to operate, the thickness of the plate layer is easy to control, the thickness of the plate layer can be regulated and controlled by regulating and controlling the sputtering arrangement of the magnesium target and the aluminum target, the metallurgical bonding between the layers of the magnesium-aluminum composite plate can be realized, and the interlayer bonding strength is good.
Drawings
Fig. 1 is a graph showing the relationship between the interface bonding strength of the magnesium-aluminum composite panel prepared by the embodiment of the invention and the temperature of the magnesium alloy matrix.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values.
Example 1
(1) Preparing a matrix: soaking a magnesium alloy matrix (with the size of phi 76.2 multiplied by 5 mm) subjected to linear cutting in an acetic acid solution with the mass concentration of 50wt% for 24 hours, removing surface oil stains, then ultrasonically cleaning the magnesium alloy matrix with deionized water for three times, wherein the time is 15min each time, the ultrasonic frequency is 100Hz, then performing single-side polishing to a mirror surface, and after polishing, respectively placing the magnesium alloy matrix in acetone, ethanol and deionized water for ultrasonic cleaning in sequence, wherein the time of ultrasonic cleaning each time is 15min, and the ultrasonic frequency is 100Hz;
(2) Then fixing the magnesium alloy substrate cleaned in the step (1) on a baffle, putting the magnesium alloy substrate into a radio frequency magnetron sputtering device sample conveying chamber for vacuumizing, wherein the vacuum degree is higher than 5 multiplied by 10 -3 Torr, and then closing a vacuum pump of the sample sending chamber;
(3) Pre-sputtering a target material: respectively pre-sputtering the magnesium target and the aluminum target in the sputtering cavity, wherein the vacuum degree of the cavity is higher than 2 multiplied by 10 during pre-sputtering -7 The Torr and the voltage are both 50V, the flow of high-purity argon gas is 20sccm, the working pressure is 3mTorr, the sputtering time is 30min, and the temperature of the cavity is cooled to 20 ℃ after the sputtering is finished; the magnesium target is pure magnesium with the purity of 99.99 percent, and the aluminum target is pure aluminum with the purity of 99.9 percent;
(4) Sample feeding: opening a gate between the sample conveying chamber and the sputtering cavity, conveying the magnesium alloy substrate prepared in the step (2) to a sample table in the sputtering cavity, and keeping the magnesium alloy substrate static on the sample table;
(5) Cleaning a sputtering cavity: opening an air inlet valve of the sputtering cavity, adjusting the flow of the high-purity argon gas to be 100sccm and the cleaning time to be 30min;
(6) Heating the matrix: heating the magnesium alloy substrate to 100 ℃ by a heater, and then adjusting the sample rotating table to rotate continuously at the rotating speed of 100rpm;
(7) Sputtering: after the heating of the substrate in the step (6) is finished, the vacuum degree of the cavity is more than or equal to 2 multiplied by 10 when the magnesium target material is sputtered -7 Torr, the voltage is 100V, the flow of high-purity argon gas is kept at 20sccm, the working pressure is 3mTorr, the sputtering time is 30min, and the deposition distance is 10cm;
the vacuum degree of the cavity is more than or equal to 2 multiplied by 10 when the aluminum target material is sputtered -7 The Torr and the voltage are 100V, the flow of high-purity argon gas is kept at 20sccm, the working pressure is 3mTorr, the sputtering time is 3h, and the deposition distance is 10cm;
(8) And (3) cooling: automatically closing the working system after sputtering is finished, and taking out the sample after the cavity is cooled to 20 ℃;
(9) Cold rolling: and (4) performing a cold rolling process with the single side of the sputtered aluminum facing upwards, and pressing down the sputtered aluminum coating by 2mm to obtain the single-side magnesium-aluminum composite plate.
(10) And (3) analysis: the interface bonding force of the magnesium-aluminum composite plate is 152MPa by adopting a microelectronic stretching instrument to stretch and measure the section of the magnesium-aluminum composite plate.
(11) The application comprises the following steps: the aluminum-magnesium composite plate has the advantages of smooth surface, good plastic forming performance and strong surface corrosion resistance, and has wide application value in the aviation, aerospace, automobile and electronic industries.
Example 2
The preparation process is the same as that of example 1, and only the heating temperature of the magnesium alloy substrate in the step (6) of example 1 is replaced by 150 ℃.
The method for testing the interface bonding force of the magnesium-aluminum composite board obtained in the embodiment is the same as that in the embodiment 1, and the interface bonding force is 202MPa.
Example 3
The preparation process is the same as that of example 1, and only the heating temperature of the magnesium alloy substrate in the step (6) of example 1 is replaced with 200 ℃.
The interface bonding force test method of the magnesium-aluminum composite board obtained in the embodiment is the same as that of the embodiment 1, and the interface bonding force is 310MPa;
example 4
The preparation process is the same as that of the embodiment 1, and only the heating temperature of the magnesium alloy matrix in the step (6) of the embodiment 1 is replaced by 250 ℃.
The method for testing the interface bonding force of the magnesium-aluminum composite plate obtained in the embodiment is the same as that of the embodiment 1, and the interface bonding force is 289MPa;
example 5
The preparation process is the same as that of the example 1, and only the heating temperature of the magnesium alloy matrix in the step (6) of the example 1 is replaced by 300 ℃.
The method for testing the interface bonding force of the magnesium-aluminum composite board obtained in the embodiment is the same as that of the embodiment 1, and the interface bonding force is 243MPa;
fig. 1 is a relationship diagram of the interface bonding strength of the magnesium-aluminum composite board prepared in the above embodiment and the temperature of the magnesium alloy substrate, and it can be seen that the influence of the heating temperature of the magnesium alloy substrate on the interface bonding strength of the prepared magnesium-aluminum composite board is relatively large, and when the heating temperature is 200 ℃, the interface bonding strength reaches a maximum of 310MPa.
Therefore, the magnesium-aluminum composite plate is obtained by sequentially sputtering and compounding the magnesium coating and the aluminum coating on the magnesium alloy substrate by utilizing the radio frequency magnetron sputtering technology and finally performing cold rolling treatment on the single surface sputtered with aluminum. The method is simple and easy to operate, the thickness of the plate layer is easy to control, the thickness of the plate layer can be regulated and controlled by regulating and controlling the sputtering arrangement of the magnesium target and the aluminum target, the metallurgical bonding between the layers of the magnesium-aluminum composite plate can be realized, and the interlayer bonding strength is good. The aluminum-magnesium composite board prepared by the invention has the advantages of smooth surface, good plastic forming performance and strong surface corrosion resistance, and has wide application value in the aviation, aerospace, automobile and electronic industries.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for preparing a magnesium-aluminum composite plate by utilizing radio frequency magnetic control is characterized by comprising the following steps:
(1) Preparing a matrix: fixing the cleaned magnesium alloy substrate on a baffle, putting the magnesium alloy substrate into a sample conveying chamber of radio frequency magnetron sputtering equipment for vacuumizing, and then closing a vacuum pump of the sample conveying chamber;
(2) Pre-sputtering: respectively carrying out pre-sputtering on the magnesium target and the aluminum target in the sputtering cavity;
(3) Sample feeding: opening a gate between the sample conveying chamber and the sputtering cavity, and conveying the magnesium alloy substrate prepared in the step (1) to a sample table in the sputtering cavity;
(4) Washing a cavity: opening an air inlet valve of the sputtering cavity, and adjusting the flow of the high-purity argon and the cleaning time to clean the cavity;
(5) Heating the matrix: turning on a heater to heat the magnesium alloy substrate, and then adjusting a sample rotating platform to rotate continuously;
(6) Sputtering: after the heating of the matrix in the step (5) is completed, the sputtering voltage, the working pressure, the sputtering time and the high-purity argon flow of the magnesium target and the aluminum target are respectively set, and the sputtering sequence set by a program is automatically executed: firstly sputtering the magnesium target material and introducing high-purity argon, closing the baffle plate after the magnesium target material sputtering is finished, then opening the baffle plate of the aluminum target material to start sputtering and introducing high-purity argon;
(7) Cold rolling: after sputtering is finished, cooling the cavity, taking out a sample, and then performing cold rolling treatment on the single surface sputtered with aluminum to obtain the magnesium-aluminum composite plate;
the vacuum degree of the cavity during sputtering of the magnesium target in the step (6) is more than or equal to 2 multiplied by 10 -7 The Torr, the voltage is 50-100V, the flow of high-purity argon gas is kept at 20sccm, the working pressure is 3mTorr, the sputtering time is 30-60 min, and the deposition distance is 10cm;
the vacuum degree of the cavity is more than or equal to 2 multiplied by 10 when the aluminum target material is sputtered -7 The Torr, the voltage is 100-200V, the flow of high-purity argon gas is kept at 20sccm, the working pressure is 3mTorr, the sputtering time is 3-6 h, and the deposition distance is 10cm;
in the step (6), the thickness of the magnesium layer sputtered by the magnesium target material is 1-3mm, and the thickness of the aluminum layer sputtered by the aluminum target material is 0.5-2mm.
2. The method for preparing the magnesium-aluminum composite board by using the radio frequency magnetron according to claim 1, wherein the cleaning of the magnesium alloy substrate in the step (1) is specifically as follows: soaking the magnesium alloy substrate subjected to linear cutting in an acetic acid solution to remove surface oil stains, then ultrasonically cleaning the magnesium alloy substrate with deionized water for three times to perform single-side polishing, and respectively placing the magnesium alloy substrate after polishing in acetone, ethanol and deionized water to perform ultrasonic cleaning in sequence.
3. The method for preparing the magnesium-aluminum composite board by utilizing the radio frequency magnetron as claimed in claim 2, wherein the size of the magnesium alloy substrate after linear cutting is phi 76.2 x 5mm, the mass concentration of the acetic acid solution is 20-50 wt%, the soaking time in the acetic acid solution is 10-24h, the ultrasonic cleaning time of deionized water before polishing is 15-30 min/time, and the ultrasonic frequency is 100Hz;
and after polishing to a mirror surface, ultrasonically cleaning the mirror surface by using acetone, ethanol and deionized water for 15-30min at 100Hz.
4. The method for preparing magnesium-aluminum composite panels by using radio frequency magnetron as claimed in claim 1, wherein the degree of vacuum of the vacuum pumping in the step (1) is higher than 5 x 10 -3 Torr。
5. The method for preparing the magnesium-aluminum composite board by using the radio frequency magnetron as claimed in claim 1, wherein the magnesium target in the step (2) is pure magnesium with a purity of 99.99%, the aluminum target is pure aluminum with a purity of 99.9%, and a vacuum degree in a sputtering chamber during the pre-sputtering is higher than 2 x 10 -7 The Torr and the voltage are 50-150V, the flow of high-purity argon is 20-40 sccm, the working pressure is 3-10 mTorr, the sputtering time is 20-30 min, and the cavity temperature is cooled to 20-30 ℃ after the sputtering is finished.
6. The method for preparing the magnesium-aluminum composite board by using the radio frequency magnetron as claimed in claim 1, wherein the flow rate of the high-purity argon in the step (4) is 100sccm, and the cleaning time is 20-30 min.
7. The method for preparing magnesium-aluminum composite board by using radio frequency magnetron as claimed in claim 1, wherein the heating in step (5) is heating the magnesium alloy substrate to 100-300 ℃, and the rotating speed of the rotating table is maintained at 100rpm.
8. The method for preparing the magnesium-aluminum composite plate by utilizing the radio frequency magnetron in the claim 1 is characterized in that in the step (7), the cavity is cooled to 20-30 ℃, the sample is taken out, in the cold rolling treatment, the coating surface sputtered with aluminum faces upwards, and the single-side cold rolling treatment is carried out, wherein the pressing amount is 1-2 mm.
9. The method for preparing the magnesium-aluminum composite board by using the radio frequency magnetron as claimed in claim 1, wherein the magnesium alloy matrix in the step (3) is kept still on a sample stage.
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