Preparation method of magnesium-aluminum composite plate reinforced by nickel intermediate layer and magnesium-aluminum composite plate

By implanting a Ni interlayer into the magnesium-aluminum composite plate and controlling the hot rolling composite and heat treatment parameters, the problem of low interfacial bonding strength of magnesium-aluminum composite materials was solved, achieving the effects of simplifying the process and improving the interfacial bonding strength.

CN118342863BActive Publication Date: 2025-12-26SOUTHWEST UNIV
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Patent Information

Application Number
CN202410529886.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-04-29
Publication Date
2025-12-26
Estimated Expiration
2044-04-29

AI Technical Summary

Technical Problem

Existing magnesium-aluminum composite materials form continuously growing hard and brittle intermetallic compounds at the interface, which reduces the interfacial bonding strength. Existing surface treatment processes increase the process flow and manufacturing difficulty.

Method used

The preparation method of Ni-intermediate layer reinforced magnesium-aluminum composite plate involves stacking magnesium plates, nickel foils and aluminum plates according to a specific thickness ratio, and controlling the rolling temperature and heat treatment parameters during hot rolling composite process to form metallurgically bonded Al-Mg diffusion layers, Al-Ni diffusion layers, Mg-Ni diffusion layers and Ni intermediate layers, which isolate the magnesium-aluminum interface reaction.

Benefits of technology

It improves the interfacial bonding strength of magnesium-aluminum composite panels, simplifies the process flow, avoids additional surface treatment, increases the contact area, and improves the interfacial bonding effect.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to the technical field of magnesium-aluminum composite materials, and particularly discloses a preparation method of a magnesium-aluminum composite plate reinforced by a Ni intermediate layer and the magnesium-aluminum composite plate, which comprises the following preparation steps: S1. providing a magnesium plate, a nickel foil and an aluminum plate, stacking the magnesium plate, the nickel foil and the aluminum plate in the mode of aluminum plate / nickel foil / magnesium plate / nickel foil / aluminum plate to obtain a laminated plate, S2. hot-rolling and compounding the laminated plate to obtain a hot-rolled plate; and S3. heat-treating the hot-rolled plate to obtain the magnesium-aluminum composite plate. In the application, the nickel foil is laminated between the magnesium plate and the aluminum plate, the magnesium plate, the aluminum plate and the nickel foil are deformed cooperatively in the hot-rolling process, Ni diffuses into Mg and Al in the deformation process, a better metallurgical combination is formed, meanwhile, due to the isolation effect of Ni on the Mg and Al interface, the defect of continuously growing brittle intermetallic compounds formed in the magnesium-aluminum combination interface in the hot-rolling deformation process is improved, and the interface combination strength of the magnesium-aluminum composite plate is significantly improved.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of magnesium-aluminum composite materials, and in particular, it relates to a preparation method of a magnesium-aluminum composite plate reinforced by a Ni intermediate layer and the magnesium-aluminum composite plate. BACKGROUND

[0002] With the rapid development of modern industry, lightweight materials are increasingly widely used in the fields of aerospace, ship transportation, electronics, automobiles, etc. Magnesium alloy and aluminum alloy are energy-rich and commonly used commercial alloys in China. Magnesium and its alloys have the advantages of high specific strength, high specific stiffness, good electromagnetic shielding performance and electrical conductivity, etc. However, due to poor corrosion resistance and poor plasticity at room temperature, magnesium alloys are not easy to process and deform, which has greatly hindered the application and development of magnesium alloys. Aluminum alloy is also one of the lightweight materials, and has a high solid solubility with magnesium alloy. By combining the two metals, the corrosion resistance and processing plasticity of magnesium alloy can be greatly improved.

[0003] At present, the preparation process of magnesium-aluminum composite plate mainly includes hot pressing, welding, casting and rolling, etc. It is found through research that various processes will produce continuously growing hard intermetallic compounds (IMC) such as Al3Mg2 and Mg17Al12 between magnesium and aluminum due to the diffusion of elements, which will greatly weaken the interface bonding performance of the material, thereby reducing the bonding strength of the interface. Therefore, how to improve the formation of continuously growing brittle intermetallic compounds in the interface layer of magnesium-aluminum composite materials has become a technical problem to be solved in the field. 17 Al 12

[0004] ​At present, in order to inhibit the continuous growth of intermetallic compounds at the magnesium-aluminum interface, the most direct method adopted by researchers is to separate the magnesium-aluminum interface by implanting an intermediate layer to improve the defects of the continuous growth of brittle intermetallic compounds. The Chinese patent document with the application number 201711007352.X discloses a continuous casting preparation method of aluminum / magnesium composite material. A nickel-aluminum alloy is formed on the surface of the magnesium core material by plasma spraying, and then aluminum melt is poured to realize the continuous casting of the aluminum / magnesium composite material with the core material being magnesium, the intermediate layer being a nickel alloy, and the cladding layer being aluminum. The formation of hard and brittle second phases in the interface area is hindered, and an aluminum / magnesium composite material with a good metallurgical bonding interface is obtained. The Chinese patent document with the application number 202210231507.2 discloses a magnesium-aluminum layered composite plate and a preparation method thereof. The composite pipe blank is prepared by centrifugal casting, which includes the following steps: first pouring the molten liquid of aluminum alloy, treating the surface of the molten liquid of aluminum alloy after it is cooled and solidified to obtain a nickel coating, and finally pouring the molten liquid of magnesium alloy. After cooling, a composite pipe blank is obtained. The composite pipe blank is pretreated to form a composite plate. Two or more composite plates of the same size are stacked and rolled in an alternating and spaced manner to obtain a magnesium-aluminum layered composite plate. A nickel layer is arranged between the two adjacent composite plates to avoid the generation of a large amount of hard and brittle intermetallic compounds at the interface of the composite plate under medium-high temperature (350-500℃), thereby facilitating the improvement of the mechanical properties of the magnesium-aluminum composite plate.

[0005] In the above related technology, in order to form a nickel layer at the interface of the magnesium-aluminum composite material, plasma spraying, chemical plating or electroplating are required to perform surface treatment on magnesium or aluminum to form a nickel coating. However, the additional surface treatment processes such as plasma spraying, chemical plating and electroplating increase the entire process flow and manufacturing difficulty. SUMMARY

[0006] The purpose of the present application is to provide a preparation method of a Ni intermediate layer reinforced magnesium-aluminum composite plate and a magnesium-aluminum composite plate, which can improve the interface bonding strength of the magnesium-aluminum composite plate, and the method is simple and easy to prepare.

[0007] In a first aspect, the present application provides a preparation method of a Ni intermediate layer reinforced magnesium-aluminum composite plate, which comprises the following preparation steps:

[0008] S1. Provide a magnesium plate, a nickel foil and an aluminum plate, stack the magnesium plate, the nickel foil and the aluminum plate in the manner of aluminum plate / nickel foil / magnesium plate / nickel foil / aluminum plate to obtain a laminated plate, and the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is (3500-4500μm):(5-50μm):(800-1200μm);

[0009] S2. hot-rolling the laminated plate to obtain a hot-rolled plate, the rolling temperature being 430-480℃, the holding time being 20-120min, and the total deformation of the hot-rolling being 50-60%;

[0010] S3. heat-treating the hot-rolled plate to obtain a magnesium-aluminum composite plate, the heat-treating temperature being 200-350℃, and the heat-treating time being 30-120min.

[0011] Optionally, in step S1, the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is (3500-4500μm):(20-50μm):(800-1200μm).

[0012] Optionally, in step S3, the heat-treating temperature is 200-270℃, and the heat-treating time is 30-120min.

[0013] Optionally, in step S2, the hot-rolled plate forms an Al-Mg diffusion layer, an Al-Ni diffusion layer, an Mg-Ni diffusion layer and a Ni intermediate layer at the bonding interface, and the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer, the Mg-Ni diffusion layer and the Ni intermediate layer is (3.0-3.2μm):(1.0-1.5μm):(1.0-1.2μm):(3.2-40μm).

[0014] Optionally, the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer, the Mg-Ni diffusion layer and the Ni intermediate layer is (3.0-3.2μm):(1.0-1.5μm):(1.0-1.2μm):(5-40μm).

[0015] Optionally, in step S2, after the hot-rolled plate is peeled, the phase structure on the aluminum plate side is Al phase or Al phase and Ni phase, and the phase structure on the magnesium plate side is Mg phase and Ni phase.

[0016] Optionally, in step S3, the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer and the Mg-Ni diffusion layer in the magnesium-aluminum composite plate is (4.8-21μm):(1.2-2.2μm):(0.8-2.2μm).

[0017] Optionally, the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer and the Mg-Ni diffusion layer in the magnesium-aluminum composite plate is (4.8-5.0μm):(1.8-2.2μm):(1.8-2.2μm).

[0018] Optionally, in step S3, after the magnesium-aluminum composite plate is peeled, the phase structure on the aluminum plate side is Al phase, Ni phase, Al 12 Mg 17The phase structure of the magnesium plate side is Mg phase, Ni phase, Al3Mg2 phase, Al 12 Mg 17 phase, Mg2Ni phase and AlNi3 phase.

[0019] In a second aspect, the present application provides a magnesium-aluminum composite plate prepared by the method for preparing a Ni-interlayer reinforced magnesium-aluminum composite plate.

[0020] In summary, the present application has at least one of the following beneficial effects:

[0021] 1. The present application provides a method for preparing a Ni-interlayer reinforced magnesium-aluminum composite plate. By implanting a Ni interlayer between the contact surfaces of the magnesium-aluminum composite plate, the foil-shaped material is easy to prepare and does not require additional introduction of a specific surface treatment process. It can be evenly laid on the surface of the plate, so that it can be relatively uniformly distributed on the interface of the magnesium-aluminum composite plate after rolling, without phenomena such as agglomeration. This increases the contact area between the foil and the magnesium-aluminum plate, increases the effective utilization area, and reduces the stress that should be borne during the subsequent rolling and stacking process. Therefore, the metal foil is more likely to produce metallurgical bonding with the interface of the aluminum plate and the magnesium plate, thereby further improving the interface bonding effect.

[0022] 2. The present application provides a method for preparing a Ni-interlayer reinforced magnesium-aluminum composite plate. When implanting a nickel foil into the magnesium-aluminum composite plate, the thickness of the Ni interlayer of the hot-rolled plate formed after rolling, as well as the temperature and deformation amount of hot rolling, will also affect its uniform distribution on the interface. The diffusion reaction between the nickel foil and the magnesium plate and the aluminum plate prevents the formation of continuous brittle intermetallic compounds between the magnesium plate and the aluminum plate. In subsequent examples, when a 25 μm Ni foil is implanted, a stronger Ni matrix peak is detected on the aluminum side of the peeling surface, which inhibits the formation of hard and brittle intermediate phases between magnesium and aluminum, thereby further improving the interface bonding strength of the magnesium-aluminum composite plate.

[0023] 3. The present application provides a method for preparing a Ni-interlayer reinforced magnesium-aluminum composite plate. After hot rolling, stress is eliminated through heat treatment, and the diffusion reaction of the Ni interlayer is further promoted, thereby significantly improving the interface bonding strength of the magnesium-aluminum composite plate. The process parameters of heat treatment have a significant effect on the diffusion reaction of the interface layer. By controlling specific heat treatment processes, magnesium-aluminum composite plates with excellent interface bonding strength can be obtained. BRIEF DESCRIPTION OF DRAWINGS

[0024] Figure 1 is the stacking mode of the laminated plate of Example 1;

[0025] Figure 2 is the SEM image of the magnesium plate side and the aluminum plate side of the hot-rolled plate after peeling of Examples 1-4;

[0026] Figure 3 are XRD patterns of the magnesium plate side and the aluminum plate side after peeling of the hot-rolled plate of Examples 1-4 and Comparative Example 1;

[0027] Figure 4 are XRD patterns of the aluminum plate side and the magnesium plate side after peeling of the magnesium-aluminum composite plate of Example 3 heat-treated at 230℃ and 350℃;

[0028] Figure 5 are SEM images and line scan images of the interface of the hot-rolled plate of Examples 1-4;

[0029] Figure 6 are SEM images and line scan images of the interface of the magnesium-aluminum composite plate of Comparative Example 1 heat-treated at 230℃ and Example 3 heat-treated at 230℃ and 350℃. DETAILED DESCRIPTION

[0030] The present application provides a preparation method of a Ni interlayer reinforced magnesium-aluminum composite plate and a magnesium-aluminum composite plate. To make the purpose, technical solutions and effects of the present application clearer and more explicit, the present application is further described in detail below. It should be understood that the specific examples described herein are only used to explain the present application and not to limit the present application.

[0031] The inventors disclosed a preparation method of a magnesium-aluminum composite plate and a magnesium-aluminum composite plate in the previous patent document with application number 202310595463.6. The surface of the magnesium plate after pretreatment is subjected to cold spray of metal powder, so that the metal powder is deposited and fixed on the surface of the magnesium plate. Then, the cold-sprayed surface of the magnesium plate and the pretreated surface of the aluminum plate are stacked, and hot-rolled to combine the metal powder with the magnesium plate and the aluminum plate, thereby further improving the interfacial bonding strength of the magnesium-aluminum composite plate. During the subsequent research, the applicant found that by changing the state of the implanted interlayer from powder to foil, only by stacking a nickel foil between the magnesium plate and the aluminum plate and hot-rolling, the nickel foil can play a role in isolating the magnesium-aluminum interface, improving the defect of continuous growth of brittle intermetallic compounds at the magnesium-aluminum interface during hot rolling. At the same time, during the hot rolling deformation process, a magnesium-nickel diffusion layer, a nickel interlayer and a nickel-aluminum diffusion layer are respectively formed on the bonding surfaces of magnesium-nickel and nickel-aluminum, which significantly improves the bonding strength of the magnesium-aluminum composite plate. Subsequent heat treatment can further improve the bonding strength of the nickel interlayer with the magnesium plate and the aluminum plate, thereby enhancing the bonding strength of the magnesium-aluminum composite plate. The preparation method of the present application is simple, does not require additional special surface treatment, and simplifies the process flow and preparation difficulty. The present application is obtained on the basis of this research.

[0032] In some embodiments of the present application, a preparation method of a Ni interlayer reinforced magnesium-aluminum composite plate is provided, comprising the following preparation steps:

[0033] S1. providing a magnesium plate, a nickel foil and an aluminum plate, and stacking the magnesium plate, the nickel foil and the aluminum plate in the order of aluminum plate / nickel foil / magnesium plate / nickel foil / aluminum plate to obtain a laminated plate, wherein the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is (3500-4500 μm):(5-50 μm):(800-1200 μm);

[0034] S2. hot-rolling the laminated plate to obtain a hot-rolled plate, wherein the rolling temperature is 430-480℃, the holding time is 20-120 min, and the total deformation amount of hot-rolling is 50-60%;

[0035] S3. heat-treating the hot-rolled plate to obtain a magnesium-aluminum composite plate, wherein the heat-treating temperature is 200-350℃, and the heat-treating time is 30-120 min.

[0036] In step S1, by controlling the thickness ratio of the magnesium plate, the aluminum plate and the nickel foil, the magnesium plate, the aluminum plate and the nickel foil can be promoted to deform cooperatively in the hot-rolling process. In the deformation process, Ni diffuses into Mg and Al to form a better metallurgical bond, so that the finally formed Ni intermediate layer can better play the effect of reinforcing the magnesium-aluminum composite plate. At the same time, due to the isolation effect of Ni at the Mg and Al interface, the defect of forming continuous brittle intermetallic compounds at the magnesium-aluminum bonding interface in the hot-rolling deformation process is improved, and the interfacial bonding strength of the magnesium-aluminum composite plate is significantly improved. Preferably, in step S1, the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is (3500-4500 μm):(20-50 μm):(800-1200 μm); more preferably, the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is (3500-4500 μm):(20-40 μm):(800-1200 μm); more preferably, the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is (3800-4200 μm):(20-30 μm):(900-1100 μm); most preferably, the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is (3900-4100 μm):(20-30 μm):(900-1100 μm).

[0037] In step S2, by controlling the rolling temperature, the holding time and the total deformation amount of rolling of the laminated plate, the hot-rolled plate prepared therefrom can obtain good microstructure and properties, refine the grains, promote the metallurgical bonding of Ni with Mg and Al, and improve the strength and plasticity and toughness of the material. Preferably, in step S2, the rolling temperature is 435-465℃, more preferably, the rolling temperature is 440-460℃; preferably, the total deformation amount of hot-rolling is 50-58%; preferably, the holding time is 30-90 min.

[0038] In step S3, by controlling the temperature and time of the heat treatment, stress is eliminated, microstructure is changed, and further diffusion of Ni into Mg and Al is promoted to form a stable metallurgical bond. Preferably, in step S3, the temperature of the heat treatment is 200-270°C, more preferably, the time of the heat treatment is 200-250°C, and more preferably, the temperature of the heat treatment is 200-240°C; preferably, the time of the heat treatment is 30-100 min, and more preferably, 40-90 min.

[0039] In some embodiments of the present application, in step S2, the hot-rolled plate forms an Al-Mg diffusion layer, an Al-Ni diffusion layer, a Mg-Ni diffusion layer, and a Ni intermediate layer at the bonding interface, and the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer, the Mg-Ni diffusion layer, and the Ni intermediate layer is: (3.0-3.2 μm):(1.0-1.5 μm):(1.0-1.2 μm):(3.2-40 μm). The Al-Mg diffusion layer, the Al-Ni diffusion layer, the Mg-Ni diffusion layer, and the Ni intermediate layer with the specific thickness ratio are advantageous for promoting the metallurgical bond between Mg-Al and Mg-Ni-Al and improving the bonding strength of the interface. Preferably, the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer, the Mg-Ni diffusion layer, and the Ni intermediate layer is: (3.0-3.2 μm):(1.0-1.5 μm):(1.0-1.2 μm):(5-40 μm).

[0040] In some embodiments of the present application, in step S2, the phase structure of the hot-rolled plate on the aluminum plate side after peeling is an Al phase or an Al phase and a Ni phase, and the phase structure of the magnesium plate side is a Mg phase and a Ni phase. By forming an Al phase or an Al phase and a Ni phase on the aluminum plate side and a Mg phase and a Ni phase on the magnesium plate side, the formation of continuous brittle intermetallic compounds on the magnesium-aluminum bonding interface is improved, and the interface bonding strength is significantly improved. Preferably, the phase structure of the hot-rolled plate on the aluminum plate side is an Al phase and a Ni phase, and the phase structure of the magnesium plate side is a Mg phase and a Ni phase.

[0041] In some embodiments of the present application, in step S3, the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer, and the Mg-Ni diffusion layer in the magnesium-aluminum composite plate is: (4.8-21 μm):(1.2-2.2 μm):(0.8-2.2 μm). By controlling the thickness of the interface bonding layer of the magnesium-aluminum composite plate after heat treatment, the interface bonding strength of the magnesium-aluminum composite plate is further improved. Preferably, the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer, and the Mg-Ni diffusion layer in the magnesium-aluminum composite plate is: (4.8-5.0 μm):(1.8-2.2 μm):(1.8-2.2 μm).

[0042] In some embodiments of the present application, in step S3, the phase structure of the aluminum plate side after the magnesium-aluminum composite plate is peeled off is Al phase, Ni phase, Al 12 Mg 17 phase, Al3Mg2 phase, the phase structure of the magnesium plate side is Mg phase, Ni phase, Al3Mg2 phase, Al 12 Mg 17 Mg2Ni phase and AlNi3 phase. By forming a small amount of discontinuous growth of metal intermetallic compound Al 12 Mg 17 Mg2 phase and AlNi3 phase at the interface of the magnesium-aluminum composite plate, the pinning effect is facilitated, and the interfacial bonding strength is further improved.

[0043] In some embodiments of the present application, a magnesium-aluminum composite plate is provided, which is prepared by the aforementioned method for preparing a Ni interlayer reinforced magnesium-aluminum composite plate.

[0044] The present application will be described below with reference to specific embodiments, and it should be noted that these embodiments are merely descriptive and do not limit the present application in any way.

[0045] Embodiment 1

[0046] A method for preparing a Ni interlayer reinforced magnesium-aluminum composite plate, comprising the following preparation steps:

[0047] S1. Provide a magnesium plate (model AZ31), a nickel foil (model N6) and an aluminum plate (model 5083), the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is 4000 μm:5 μm:1000 μm, stack the magnesium plate, the aluminum plate and the nickel foil to obtain a laminated plate, the width and length of the laminated plate is 100mm×200mm, specifically comprising the following steps:

[0048] S1-1. Roughen the pre-bonding surfaces of the magnesium plate and the aluminum plate respectively: uniformly polish the pre-bonding surfaces of the cut magnesium plate and the aluminum plate using a steel wire brush mounted on an electric drill to remove the oxidation layer and passivation layer on the surface of the plate and expose the fresh metal, then manually polish with a steel wire brush to brush out a small groove in the shape of a rice character;

[0049] S1-2. Clean the surfaces of the magnesium plate, the aluminum plate and the nickel foil respectively, first use 3% HCl aqueous solution for room temperature pickling, after pickling, clean with pure water, then use 3% NaOH aqueous solution for room temperature alkaline cleaning, after alkaline cleaning, clean with pure water, finally clean with anhydrous ethanol and blow dry;

[0050] S1-3. As shown in Figure 1 , after the magnesium plate, the nickel foil and the aluminum plate are stacked in the order of aluminum plate / nickel foil / magnesium plate / nickel foil / aluminum plate to obtain a laminated plate, the laminated plate is fixed at the front end before rolling by using rivets.

[0051] S2. The laminated plate prepared in step S1 was subjected to hot rolling to obtain a hot-rolled plate, the hot rolling was carried out by synchronous single pass rolling, the rolling temperature was 450℃, the holding time was 45 min, the rolling roller speed was 2 m / min, and the total deformation amount of hot rolling was 53%.

[0052] S3. The hot-rolled plate prepared in step S2 was subjected to heat treatment at different temperatures, respectively, the heat treatment temperature was 200℃, 230℃, 250℃, 270℃, 350℃, respectively, the heat treatment time was 60 min, and a magnesium-aluminum composite plate was prepared.

[0053] Example 2

[0054] Example 2 differs from Example 1 in that the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate provided in step S1 of Example 2 is 4000 μm: 10 μm: 1000 μm, and the remaining preparation steps are the same as those of Example 1.

[0055] Example 3

[0056] Example 3 differs from Example 1 in that the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate provided in step S1 of Example 3 is 4000 μm: 25 μm: 1000 μm, and the remaining preparation steps are the same as those of Example 1.

[0057] Example 4

[0058] Example 4 differs from Example 1 in that the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate provided in step S1 of Example 4 is 4000 μm: 50 μm: 1000 μm, and the remaining preparation steps are the same as those of Example 1.

[0059] Comparative Example 1

[0060] Comparative Example 1 differs from Example 1 in that only a magnesium plate and an aluminum plate are provided in step S1 of Comparative Example 1, no nickel foil is provided, the thickness ratio of the magnesium plate and the aluminum plate is 4000 μm: 1000 μm, and the magnesium plate and the aluminum plate are stacked in the manner of aluminum plate / magnesium plate / aluminum plate to obtain a laminated plate, and the remaining preparation steps are the same as those of Example 1.

[0061] Performance test and structure characterization:

[0062] 1. The interface bonding strength of the hot-rolled plate prepared in step S2 and the magnesium-aluminum composite plate prepared in step S3 of Example 1-4 and Comparative Example 1 was tested by sampling. The interface bonding strength was tested by peeling test. The sampling size was 10x80mm. The Al side of the front end of the sample was peeled off about 20mm. The Al+Mg of the other side was turned 90° to form a T-shaped sample. The peeled two sides were clamped by a universal testing machine. The sample was peeled off until it was completely peeled off. The maximum force F required for complete peeling was measured. The peeling strength P was calculated according to the formula: P=F / d, where d was the width of the T-shaped sample. The test results are shown in Table 1.

[0063] 2. The magnesium plate side and the aluminum plate side of the hot-rolled plate of Example 1-4 were tested by SEM. The test results are shown in Table 2. Figure 2

[0064] 3. The magnesium plate side and the aluminum plate side of the hot-rolled plate of Example 1-4 and Comparative Example 1 were tested by XRD. The test results are shown in Table 3. Figure 3

[0065] 4. The magnesium plate side and the aluminum plate side of the magnesium-aluminum composite plate of Example 3 were tested by XRD. The test results are shown in Table 4. Figure 4

[0066] 5. The interface of the hot-rolled plate of Example 1-4 was analyzed by element scanning. The scanning results are shown in Table 2. The analysis results of element scanning are shown in Table 2. Figure 5

[0067] 6. The interface of the magnesium-aluminum composite plate of Example 3 and Comparative Example 1 was analyzed by element scanning. The test results are shown in Table 3. The analysis results of element scanning are shown in Table 3. Figure 6

[0068] Table 1. Interface bonding strength of the hot-rolled plate and the magnesium-aluminum composite plate of Example 1-4 and Comparative Example 1

[0069]

[0070]

[0071] ​​​​​As can be seen from Table 1, the properties of the hot-rolled plate prepared in Examples 2-4 are obviously increased compared with those of Comparative Example 1. With the increase of the thickness of the Ni foil, the interfacial bonding strength of the hot-rolled plate gradually increases. When the thickness of the Ni foil is increased to 25 μm in Example 3, the interfacial bonding strength of the hot-rolled plate is the highest. With the further increase of the thickness of the Ni foil, the interfacial bonding strength of the hot-rolled plate decreases. In addition, the interfacial bonding strength of the magnesium-aluminum composite plate prepared by heat treatment of the hot-rolled plate can be obviously increased. With the increase of the heat treatment temperature, the interfacial bonding strength increases. In Examples 1-4, when the heat treatment temperature is increased to 230 °C, the interfacial bonding strength is the best. With the further increase of the heat treatment temperature, the interfacial bonding strength decreases.

[0072] Figure 2 (a) (b) are SEM images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Example 1 after peeling, respectively. From (a), it can be seen that the Ni layer is flat and adheres to the magnesium plate surface after hot rolling. From (b), it can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (a) (b) are SEM images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Example 1 after peeling, respectively. From (a), it can be seen that the Ni layer is flat and adheres to the magnesium plate surface after hot rolling. From (b), it can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (b) can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (c) (d) are SEM images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Example 2 after peeling, respectively. From (c), it can be seen that the Ni foil is deformed after hot rolling, and the Ni layer is in the form of a winding river and adheres to the magnesium plate surface. From (d), it can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (c) (d) are SEM images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Example 2 after peeling, respectively. From (c), it can be seen that the Ni foil is deformed after hot rolling, and the Ni layer is in the form of a winding river and adheres to the magnesium plate surface. From (d), it can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (d) can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (e) (f) are SEM images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Example 3 after peeling, respectively. From (e), it can be seen that the Ni foil is more obviously deformed after hot rolling, and the Ni layer is in the form of a bifurcated tree and adheres to the magnesium plate surface. From (f), it can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (e) (f) are SEM images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Example 3 after peeling, respectively. From (e), it can be seen that the Ni foil is more obviously deformed after hot rolling, and the Ni layer is in the form of a bifurcated tree and adheres to the magnesium plate surface. From (f), it can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (f) can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (g) (h) are SEM images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Example 4 after peeling, respectively. From (g), it can be seen that the Ni foil is partially fractured after hot rolling, and the Ni layer is in the form of a parallel arranged tree trunk and adheres to the magnesium plate surface. From (h), it can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (g) (h) are SEM images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Example 4 after peeling, respectively. From (g), it can be seen that the Ni foil is partially fractured after hot rolling, and the Ni layer is in the form of a parallel arranged tree trunk and adheres to the magnesium plate surface. From (h), it can be seen that the aluminum plate surface does not see the Ni layer adhering. Figure 2 (h) can be seen that the aluminum plate surface does not see the Ni layer adhering.

[0073] Figure 3 (a) (b) are XRD images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Examples 1-4 and Comparative Example 1 after peeling, respectively. From (a), it can be seen that only the Mg phase is detected on the magnesium plate side of Comparative Example 1, and the Mg phase and the Ni phase are detected on the magnesium plate side of Examples 1-4. From (b), it can be seen that only the Al phase is detected on the aluminum plate side of Comparative Example 1, and the Al phase and the Ni phase are detected on the aluminum plate side of Examples 1-4. Figure 3 (a) (b) are XRD images of the magnesium plate side and the aluminum plate side interfaces of the hot-rolled plate of Examples 1-4 and Comparative Example 1 after peeling, respectively. From (a), it can be seen that only the Mg phase is detected on the magnesium plate side of Comparative Example 1, and the Mg phase and the Ni phase are detected on the magnesium plate side of Examples 1-4. From (b), it can be seen that only the Al phase is detected on the aluminum plate side of Comparative Example 1, and the Al phase and the Ni phase are detected on the aluminum plate side of Examples 1-4. Figure 3(b) It can be seen that only Al phase was detected on the side of the aluminum plate of Comparative Example 1, Examples 1-2 and Example 4, and Al phase and Ni phase were detected on the side of the aluminum plate of Example 3.

[0074] Figure 4 (a) (b) are XRD patterns of the interface between the aluminum plate and the magnesium plate after peeling of the magnesium-aluminum composite plate heat-treated at 230°C in Example 3, respectively, Figure 4 (c) (d) are XRD patterns of the interface between the aluminum plate and the magnesium plate after peeling of the magnesium-aluminum composite plate heat-treated at 350°C in Example 3. From Figure 4 It can be seen in (a) that Al phase, Ni phase, Al 12 Mg 17 phase and Al3Mg2 phase were detected on the side of the aluminum plate of the magnesium-aluminum composite plate heat-treated at 230°C in Example 3, from Figure 4 It can be seen in (b) that Mg phase, Ni phase, Al3Mg2 phase, Al 12 Mg 17 phase, Mg2Ni phase and AlNi3 phase were detected on the side of the magnesium plate. Figure 4 It can be seen in (c) that Al phase, Mg phase, Al 12 Mg 17 phase, Al3Mg2 phase and Mg2Ni phase were detected on the side of the aluminum plate of the magnesium-aluminum composite plate heat-treated at 350°C in Example 3, from Figure 4 It can be seen in (d) that Mg phase, Ni phase, Al3Mg2 phase, Al 12 Mg 17 phase, Mg2Ni phase and AlNi3 phase were detected on the side of the magnesium plate of the magnesium-aluminum composite plate heat-treated at 350°C in Example 3.

[0075] Table 2. Thickness of each layer of the interface of the hot-rolled plate of Examples 1-4 and Comparative Example 1

[0076]

[0077] It can be seen from Figure 5 and Table 2 that the thickness of the Al-Mg diffusion layer of the interface of the hot-rolled plate of Examples 1-4 decreased compared with that of Comparative Example 1, Al-Ni diffusion layer was formed at the aluminum-nickel interface in Examples 1-4, and the thickness of the Al-Ni diffusion layer was the largest when the thickness of the nickel foil was 25 μm in Example 3, Mg-Ni diffusion layer was formed at the magnesium-nickel interface, and the thickness of the Mg-Ni diffusion layer did not change significantly, and the thickness of the Ni intermediate layer increased with the increase of the thickness of the nickel foil, and the thickness of the Ni intermediate layer decreased significantly in Example 3.

[0078] Table 3. Thickness of each diffusion layer of the interface of the magnesium-aluminum composite plate after heat treatment of Example 3 and Comparative Example 1

[0079]

[0080] In combination Figure 6 As can be seen from Table 2 and Table 3, the hot-rolled plate of Comparative Example 1 obtains the magnesium-aluminum composite plate after heat treatment at 230 DEG C, and the Al-Mg diffusion layer at the magnesium-aluminum interface of the magnesium-aluminum composite plate is obviously increased compared with before heat treatment; the hot-rolled plate of Example 3 obtains the magnesium-aluminum composite plate after heat treatment at 230 DEG C, and the thickness of the Al-Mg diffusion layer, the Al-Ni diffusion layer and the Mg-Ni diffusion layer are all increased compared with before heat treatment; after heat treatment at 350 DEG C, the thickness of the Al-Mg diffusion layer is significantly increased, while the thickness of the Al-Ni diffusion layer and the Mg-Ni diffusion layer does not change obviously compared with before heat treatment.

[0081] The above are preferred embodiments of the present application, and are not intended to limit the protection scope of the present application, so: any equivalent changes made in the structure, shape, principle of the present application should be covered within the protection scope of the present application.

Claims

1. A method for preparing a Ni interlayer reinforced magnesium-aluminum composite panel, characterized in that, The preparation method comprises the following steps: S1. providing a magnesium plate, a nickel foil and an aluminum plate, stacking the magnesium plate, the nickel foil and the aluminum plate in the order of aluminum plate / nickel foil / magnesium plate / nickel foil / aluminum plate to obtain a laminated plate, wherein the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is (3500-4500 μm):(5-50 μm):(800-1200 μm); S2. hot-rolling the laminated plate to obtain a hot-rolled plate, wherein the rolling temperature is 430-480 ℃, the holding time is 20-120 min, and the total deformation of hot-rolling is 50-60%; in step S2, the hot-rolled plate forms an Al-Mg diffusion layer, an Al-Ni diffusion layer, an Mg-Ni diffusion layer and a nickel intermediate layer at the bonding interface, and the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer, the Mg-Ni diffusion layer and the nickel intermediate layer is (3.0-3.2 μm):(1.0-1.5 μm):(1.0-1.2 μm):(3.2-40 μm); S3. heat-treating the hot-rolled plate to obtain a magnesium-aluminum composite plate, wherein the heat-treating temperature is 200-350 ℃, and the heat-treating time is 30-120 min.

2. The method for preparing the Ni interlayer reinforced magnesium-aluminum composite plate according to claim 1, characterized in that, In step S1, the thickness ratio of the magnesium plate, the nickel foil and the aluminum plate is (3500-4500 μm):(20-50 μm):(800-1200 μm).

3. The method of producing a Ni-interlayer reinforced magnesium-aluminum composite sheet according to claim 1 or 2, characterized in that, In step S3, the heat-treating temperature is 200-270 ℃, and the heat-treating time is 30-120 min.

4. The method for preparing the Ni interlayer reinforced magnesium-aluminum composite plate according to claim 1, characterized in that, In step S2, the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer, the Mg-Ni diffusion layer and the nickel intermediate layer is (3.0-3.2 μm):(1.0-1.5 μm):(1.0-1.2 μm):(5-40 μm).

5. The method for preparing the Ni interlayer reinforced magnesium-aluminum composite plate according to claim 1, characterized in that, In step S2, after the hot-rolled plate is peeled, the phase structure on the aluminum plate side is an Al phase or an Al phase and a Ni phase, and the phase structure on the magnesium plate side is an Mg phase and a Ni phase.

6. The method for preparing the Ni interlayer reinforced magnesium-aluminum composite plate according to claim 4, characterized in that, In step S3, the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer and the Mg-Ni diffusion layer in the magnesium-aluminum composite plate is (4.8-21 μm):(1.2-2.2 μm):(0.8-2.2 μm).

7. The method for preparing a Ni-intermediate layer reinforced magnesium-aluminum composite plate according to claim 6, characterized in that, In step S3, the thickness ratio of the Al-Mg diffusion layer, the Al-Ni diffusion layer and the Mg-Ni diffusion layer in the magnesium-aluminum composite plate is (4.8-5.0 μm):(1.8-2.2 μm):(1.8-2.2 μm).

8. The method for preparing a Ni-intermediate layer reinforced magnesium-aluminum composite plate according to claim 1, characterized in that, In step S3, the phase structure of the aluminum plate side after the magnesium-aluminum composite plate is peeled is Al phase, Ni phase, Al 12 Mg 17 phase, and Al3Mg2 phase, and the phase structure of the magnesium plate side is Mg phase, Ni phase, Al3Mg2 phase, Al 12 Mg 17 phase, Mg2Ni phase, and AlNi3 phase.

9. A magnesium-aluminum composite plate prepared by the preparation method of the Ni intermediate layer reinforced magnesium-aluminum composite plate according to any one of claims 1-8.

Citation Information

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