Cu-Si3N4-FeCoCrNiMn nano layered composite material and preparation method thereof

Abstract

The invention discloses a Cu-Si3N4-FeCoCrNiMn nano layered composite material and a preparation method thereof, the Cu-Si3N4-FeCoCrNiMn nano layered composite material is characterized in that the Cu-Si3N4-FeCoCrNiMn nano layered composite material comprises a plurality of groups of layered composite units which are sequentially compounded and stacked, each group of layered composite units is formed by sequentially compounding and stacking a Cu film, a Si3N4 film and a FeCoCrNiMn film, the thickness of the Cu film is 30-100 nm, the thickness of the Si3N4 film is 5-15 nm, and the thickness of the FeCoCrNiMn film is 20-60 nm; the Cu-Si3N4-FeCoCrNiMn nano layered composite material has the advantages that the Cu-Si3N4-FeCoCrNiMn nano layered composite material is combined with high thermal conductivity / electrical conductivity of Cu, high hardness and high temperature resistance of Si3N4 ceramic and excellent mechanical properties of FeCoCrNiMn high-entropy alloy, and multi-scale synergistic enhancement is realized. Wherein the Cu layer serves as a plastic buffer phase to passivate crack propagation and relieve interface stress concentration, and the Si3N4 layer can effectively pinning dislocation motion and inhibit high-temperature grain boundary slippage, so that the high-temperature stability and wear resistance of the material are remarkably improved. And moreover, the nano layered structure can regulate and control the average free path of dislocation, the thickness size effect is fully utilized, and good toughness is kept while the strength is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of composite materials, and particularly to a Cu-Si3N4-FeCoCrNiMn nanolayered composite material and a preparation method thereof. Background Art

[0002] In the research and application of structural materials, achieving the coordinated improvement of high strength and high ductility has always been one of the core goals. However, due to the differences in load-bearing mechanisms during material deformation, strength and ductility often exhibit a "strength-ductility trade-off" effect where one increases while the other decreases. Traditional strengthening methods, such as grain refinement, solid solution strengthening, or precipitation hardening, although can significantly improve the strength of materials, often result in a significant decrease in plasticity and toughness, limiting their serviceability under extreme working conditions. Therefore, how to break through this inherent limitation through microstructural design and develop advanced structural materials with both high strength and high ductility has become an important development direction in the field of materials science.

[0003] As a typical face-centered cubic (FCC) structured high-entropy alloy, FeCoCrNiMn exhibits excellent low-temperature toughness, good ductility, and strong-toughness matching performance, showing good mechanical stability under extreme environments. This benefits from its complex multi-component composition and high mixing entropy effect, which can effectively delay the initiation and propagation of cracks during plastic deformation. However, this high-entropy alloy also has a series of problems that need to be solved urgently: First, its room-temperature strength is relatively low (about 500 MPa), unable to meet the requirements of high-strength structural applications; Second, under high-temperature conditions, the FCC structure is prone to grain boundary softening and diffusion creep deformation, resulting in a rapid deterioration of high-temperature mechanical properties; In addition, the lack of a second-phase strengthening mechanism makes its wear resistance limited; In terms of functionality, such as electrical conductivity, thermal conductivity, and radiation resistance, it also shows deficiencies due to its single solid-solution structure. The above problems severely restrict the application of FeCoCrNiMn high-entropy alloy in key fields such as aerospace, nuclear energy, and high-temperature equipment.

[0004] Due to its controllable layer thickness and interfacial characteristics, the nanolayered composite structure is considered one of the effective strategies to break the strength-ductility trade-off. By precisely regulating the layer thickness and interfacial structure, nanolayered materials can restrict and regulate dislocation motion, enhancing the material while retaining or even improving ductility. For example, when the layer thickness is relatively large (tens to hundreds of nanometers), dislocations accumulate between layers to form a strengthening effect similar to the Hall-Petch mechanism; while when the layer thickness drops below the critical value, the material exhibits an "interface barrier mechanism" dominated by the interface, making the strength tend to be stable and no longer decrease. At the same time, the processes of dislocation storage and annihilation at the interface also help release local stress concentrations and improve plasticity. Research on FeCoCrNiMn-based nanolayered composite structures shows that such materials can significantly enhance their strength by refining the layer thickness while retaining the plasticity of high-entropy alloys. However, nanolayered structures also face several challenges, such as interfacial reactions, insufficient thermal stability, and difficulties in matching the thermal physical properties of different components in multiphase systems, which limit their engineering applications. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a Cu-Si3N4-FeCoCrNiMn nanolayered composite material and its preparation method, which realizes the coordinated optimization of high strength, high toughness, excellent high-temperature performance and multi-function by constructing an alternating nanolayered structure of Cu / Si3N4 / high-entropy alloy, meeting the requirements of high-performance composite materials in fields such as aerospace, nuclear energy, and microelectronics.

[0006] The technical solution adopted by the present invention to solve the above technical problem is: The Cu-Si3N4-FeCoCrNiMn nanolayered composite material includes multiple groups of layered composite units stacked in sequence. Each group of layered composite units is composed of a Cu film, a Si3N4 film, and a FeCoCrNiMn film stacked in sequence, and the thickness of the Cu film is 30 - 100 nm, the thickness of the Si3N4 film is 5 - 15 nm, and the thickness of the FeCoCrNiMn film is 20 - 60 nm.

[0007] Further, the thickness of the Cu film is 50 - 70 nm, the thickness of the Si3N4 film is 6 - 10 nm, and the thickness of the FeCoCrNiMn film is 30 - 50 nm.

[0008] Further, the thickness of the Cu film is 60 nm, the thickness of the Si3N4 film is 8 nm, and the thickness of the FeCoCrNiMn film is 40 nm.

[0009] Further, there are 6 - 10 groups of the layered composite units.

[0010] Further, there are 7 groups of the layered composite units.

[0011] Preparation method of Cu-Si3N4-FeCoCrNiMn nanolayered composite material, comprising the following specific steps: (1) Fix a Cu target, an FeCoCrNiMn target and an Si3N4 target on the target head of a magnetron sputtering instrument respectively; (2) Reduce the pressure in the sputtering cavity of the magnetron sputtering instrument to 5×10 -4 Pa, and simultaneously introduce argon as a sputtering medium, and perform pre-sputtering on the Cu target, the FeCoCrNiMn target and the Si3N4 target respectively to remove the oxide layer or adsorbed impurities on the target surface; (3) First deposit a Cu thin film on the Si substrate, control the argon flow rate to be 50 sccm, the sputtering gas pressure to be 0.7-1.8 Pa, the power supply power to be 120 W, and the deposition time to be 5 minutes, so that the deposition thickness of the Cu thin film reaches 30-100 nm; (4) Then deposit an Si3N4 thin film on the Cu thin film, control the argon flow rate to be 50 sccm, the sputtering gas pressure to be 1.5 Pa, the power supply power to be 90 W, and the deposition time to be 2-5 minutes, so that the deposition thickness of the Si3N4 thin film reaches 5-15 nm; (5) Finally, deposit an FeCoCrNiMn thin film on the Si3N4 thin film, control the argon flow rate to be 60 sccm, the sputtering gas pressure to be 1.3-2.3 Pa, the power supply power to be 120 W, and the deposition time to be 5 minutes, so that the deposition thickness of the FeCoCrNiMn thin film reaches 20-60 nm, thereby obtaining a set of layered composite units; (6) Then deposit a Cu thin film on the FeCoCrNiMn thin film of the layered composite unit, and repeat steps (3)-(5) 5-9 times in a cycle to obtain the Cu-Si3N4-FeCoCrNiMn nanolayered composite material.

[0012] Preferably, in the step (1), the purity of the Cu target is 99.9999%, the purity of the FeCoCrNiMn target is 99.95%, and the purity of the Si3N4 target is 99.9%.

[0013] Preferably, in the step (1), the Cu target and the FeCoCrNiMn target are respectively fixed on the first permanent magnet target head and the strong magnet target head connected to the DC power supply, and the Si3N4 target is fixed on the second permanent magnet target head connected to the RF power supply.

[0014] Compared with the prior art, the advantages of the present invention are as follows: The Cu-Si3N4-FeCoCrNiMn nanolayered composite material combines the high thermal / electrical conductivity of Cu, the high hardness and high temperature resistance of the Si3N4 ceramic, and the excellent mechanical properties of the FeCoCrNiMn high-entropy alloy to achieve multi-scale synergistic strengthening. Among them: The Cu layer serves as a plastic buffer phase to passivate crack propagation and relieve interfacial stress concentration. The Si3N4 layer can effectively pin the movement of dislocations, inhibit high-temperature grain boundary sliding, and significantly improve the high-temperature stability, wear resistance, hardness, and corrosion resistance of the material. Moreover, the nanolayered structure can regulate the mean free path of dislocations, make full use of the thickness size effect, and maintain good toughness while increasing the strength. In addition, in terms of functional characteristics, the introduction of the Cu layer can provide an efficient conductive / thermal conduction path, and the insulating and radiation-resistant characteristics of Si3N4 can make up for the deficiencies of the high-entropy alloy in electromagnetic shielding and nuclear applications, thus realizing the multi-functional design of the material. Brief Description of the Drawings

[0015] Figure 1 It is a schematic cross-sectional view of the Cu-Si3N4-FeCoCrNiMn nanolayered composite material of the present invention; Figure 2 It is a comparative graph of the thermogravimetric analysis results of the Cu-FeCoCrNiMn and Cu-Si3N4-FeCoCrNiMn nanolayered composite materials of the present invention; Figure 3 It is a comparative graph of the experimental results of the potentiodynamic electrochemical corrosion method for high-speed steel, the Cu-FeCoCrNiMn thin film deposited on high-speed steel, and the Cu-Si3N4-FeCoCrNiMn thin film of the present invention respectively; Figure 4 It is a comparative graph of the test results of the Young's modulus and hardness of the Cu-FeCoCrNiMn and Cu-Si3N4-FeCoCrNiMn nanolayered composite materials of the present invention. Detailed Description of the Embodiments

[0016] The present invention will be further described in detail below in conjunction with the embodiments in the drawings.

[0017] Embodiment 1: The Cu-Si3N4-FeCoCrNiMn nanolayered composite material includes 7 groups of sequentially compounded and stacked layered composite units. Each group of layered composite units is composed of a Cu film, a Si3N4 film, and a FeCoCrNiMn film sequentially compounded and stacked. The thickness of the Cu film is 60 nm, the thickness of the Si3N4 film is 8 nm, and the thickness of the FeCoCrNiMn film is 40 nm.

[0018] In the first embodiment above, the thickness of the Cu film can be selected within the range of 30 - 100 nm, preferably 50 - 70 nm, and the optimal thickness is 60 nm. This not only ensures that the Cu film has good electrical and thermal conductivity but also provides the necessary plastic deformation ability; the thickness of the Si3N4 film can be selected within the range of 5 - 15 nm, preferably 6 - 10 nm, and the optimal thickness is 8 nm. Strictly setting the thickness of the Si3N4 film can avoid an increase in brittleness while ensuring the interface strengthening effect; the thickness of the FeCoCrNiMn film can be selected within the range of 20 - 60 nm, preferably 30 - 50 nm, and the optimal thickness is 40 nm. Setting the thickness of the FeCoCrNiMn film can give full play to the strengthening and toughening characteristics of the high-entropy alloy.

[0019] In addition, in the above nano-layered composite material, the number of groups of layered composite units can be selected within the range of 6 - 10 groups, preferably 7 groups; setting the number of groups of layered composite units can significantly improve the interface effect and mechanical properties of the Cu-Si3N4-FeCoCrNiMn nano-layered composite material, achieve the synergistic strengthening effect of the nano-layered structure, and at the same time avoid the accumulation of interface defects, ensuring the density and stability of the material.

[0020] By cutting the above Cu-Si3N4-FeCoCrNiMn nano-layered composite material with FIB and observing it with TEM, a nano-layered composite structure with uniform and alternating distribution of Cu, Si3N4, and FeCoCrNiMn three phases and clear interfaces can be seen, as Figure 1 shown.

[0021] Embodiment 2: A preparation method of a Cu-Si3N4-FeCoCrNiMn nano-layered composite material, including the following specific steps: (1). Fix a Cu target, a FeCoCrNiMn target, and a Si3N4 target on the target head of a magnetron sputtering instrument respectively, where: the purity of the Cu target is 99.9999%, the purity of the FeCoCrNiMn target is 99.95%, and the purity of the Si3N4 target is 99.9%; and fix the Cu target and the FeCoCrNiMn target on the first permanent magnet target head and the strong magnet target head connected to the DC power supply respectively, and fix the Si3N4 target on the second permanent magnet target head connected to the RF power supply; (2). Reduce the pressure in the sputtering cavity of the magnetron sputtering instrument to 5×10 -4 Pa, and at the same time introduce argon as the sputtering medium, and pre-sputter the Cu target, the FeCoCrNiMn target, and the Si3N4 target respectively to remove the oxide layer or adsorbed impurities on the target surface; (3) First, deposit a Cu thin film on the Si substrate, controlling the argon flow rate to be 50 sccm, the sputtering gas pressure to be 0.7 Pa, the DC power supply power to be 120 W, and the deposition time to be 5 minutes, so that the deposition thickness of the Cu thin film reaches 60 nm; (4) Then, deposit a Si3N4 thin film on the Cu thin film, controlling the argon flow rate to be 50 sccm, the sputtering gas pressure to be 1.5 Pa, the RF power supply power to be 90 W, and the deposition time to be 4 minutes, so that the deposition thickness of the Si3N4 thin film reaches 8 nm; (5) Finally, deposit a FeCoCrNiMn thin film on the Si3N4 thin film, controlling the argon flow rate to be 60 sccm, the sputtering gas pressure to be 1.3 Pa, the DC power supply power to be 120 W, and the deposition time to be 5 minutes, so that the deposition thickness of the FeCoCrNiMn thin film reaches 40 nm, thereby obtaining a group of layered composite units; (6) Then, deposit a Cu thin film on the FeCoCrNiMn thin film of the layered composite unit, and repeat steps (3) - (5) 6 times to obtain a Cu-Si3N4-FeCoCrNiMn nanolayered composite material.

[0022] In the above-mentioned second embodiment, a three-target magnetron sputtering instrument with the model TRP450 can be used.

[0023] Perform the following performance verification on the Cu-Si3N4-FeCoCrNiMn nanolayered composite material prepared by this method.

[0024] (I) Respectively perform thermogravimetric analysis (TG curve) on the Cu-FeCoCrNiMn and Cu-Si3N4-FeCoCrNiMn nanolayered composite materials. As Figure 2 shown, the results show that the mass of the Cu-FeCoCrNiMn composite material begins to increase at 622.7 °C and reaches mass balance at 788.6 °C. When the temperature rises to 839.2 °C, the mass of the Cu-FeCoCrNiMn sample begins to decrease and finally stabilizes at 918.4 °C. This indicates that in the case of not adding an interfacial material, the thermal stability of the Cu-FeCoCrNiMn composite material under high-temperature conditions is weak, showing obvious oxidation and decomposition behaviors.

[0025] After adding the Si3N4 interfacial layer between the Cu film and the FeCoCrNiMn film, the thermal stability of the Cu-Si3N4-FeCoCrNiMn nanolayered composite material is significantly improved. When the deposition time of Si3N4 is 2 minutes, the critical temperature of the mass increase of the Cu-Si3N4-FeCoCrNiMn composite material is postponed to 686 °C, and the temperature at which the mass begins to decrease is postponed to 897 °C. At the same time, the amplitude of the mass increase is significantly reduced. This indicates that the Si3N4 interfacial layer can effectively delay the chemical reaction between Cu and FeCoCrNiMn and inhibit the oxidation process. When the deposition time of Si3N4 is extended to 3 minutes, the critical temperature of the mass increase is postponed to 691.6 °C, the critical temperature at which the mass begins to decrease is further postponed to 904.5 °C, and the amplitude of the mass increase is further reduced; especially when the deposition time is extended to 4 minutes, the mass of the Cu-Si3N4-FeCoCrNiMn composite material hardly changes significantly, indicating that it has more excellent thermal stability in a high-temperature environment. Thus, it can be seen that the Si3N4 interfacial layer plays an important role in suppressing the high-temperature oxidation behavior of the layered composite structure and improving the thermal stability. And as the deposition time of Si3N4 is extended, the shielding effect of the Si3N4 interfacial material becomes more significant, effectively reducing the reaction between the Cu and FeCoCrNiMn layers. Its main mechanism of action is to form a physical and chemical barrier to prevent the diffusion of oxygen and the direct reaction between Cu and FeCoCrNiMn under high-temperature conditions. In addition, the high melting point and low diffusion coefficient of the Si3N4 interfacial layer are also the key factors for its excellent thermal stability at high temperatures. These characteristics effectively reduce the activity of the chemical reaction at the interface, thus significantly improving the thermal performance of the layered composite structure. By optimizing the thickness of the Si3N4 layer, the fine regulation of the thermal stability of the layered composite structure can be achieved. However, the thickness of the interfacial layer needs to be appropriately controlled. Although a thicker Si3N4 layer can further improve the thermal stability, an overly thick interfacial material will have a potential impact on the mechanical properties and surface microtopography of the composite material.

[0026] (2) Test the corrosion resistance of the Cu-Si3N4-FeCoCrNiMn nanolayered composite material, specifically: use the potentiodynamic electrochemical corrosion method to test high-speed steel (HSS), the Cu-FeCoCrNiMn thin film deposited on HSS, and the Cu-Si3N4-FeCoCrNiMn thin films with different Si3N4 deposition times respectively. The results are shown in Figure 3. Figure 3The Tafel curves of each material are shown in (a). It can be seen from the figure that the corrosion potential (Ecorr) of HSS is -0.6114 V and the corrosion current density (Jcorr) is -5.73 A / cm², showing relatively low stability and a slow dissolution rate. The corrosion potential of the Cu-FeCoCrNiMn film is significantly increased to -0.5226 V, indicating higher chemical stability in 3.5% NaCl solution. However, its corrosion current density is slightly increased compared with that of HSS, reflecting that while improving the passivation performance of the material surface, there may be surface defects or other factors leading to enhanced local electrochemical reactions, resulting in the failure to effectively slow down the dissolution rate. And Si3N4 can effectively improve the chemical stability of HSS in 3.5% NaCl solution. From Figure 3 It can be seen from the variation law of the corrosion potential (red curve) and corrosion current density (black curve) of different samples with the Si3N4 deposition time in (b) that as the Si3N4 deposition time increases, the corrosion potential (Ecorr) shows a trend of first decreasing, then rising and tending to be stable. It reaches the lowest value at 2 min of deposition, and significantly increases at 4 min and 5 min, indicating that the Si3N4 film may have incomplete coverage or defects in the initial stage of deposition. However, as the deposition time increases, a dense and uniform protective layer gradually forms on the surface, improving the chemical stability of the material. At the same time, the corrosion current density (Jcorr) shows a trend of "first increasing and then decreasing", reaching the maximum value at 3 min, and then significantly decreasing at 4 min and 5 min, indicating that the protective effect of the film is insufficient when the deposition time is short, resulting in an accelerated dissolution rate of the material. As the deposition time increases, the formation of the passivation film effectively inhibits the corrosion reaction. Overall, the Cu-Si3N4-FeCoCrNiMn nanolayered composite material with a 4-min Si3N4 film deposition achieves a better balance in terms of potential and current density, significantly improving the corrosion resistance of the Cu-FeCoCrNiMn film.

[0027] (3) The Young's modulus and hardness of the Cu-FeCoCrNiMn and Cu-Si3N4-FeCoCrNiMn nanolayered composite materials are tested respectively, as Figure 4As shown, the Young's modulus (black curve) of the Cu-FeCoCrNiMn nanolayered composite material is approximately 64 GPa, and the hardness (red curve) is approximately 1.9 GPa. With the extension of the Si3N4 deposition time, both the Young's modulus and hardness of the Cu-Si3N4-FeCoCrNiMn nanolayered composite material show an obvious increasing trend. As the Si3N4 deposition time gradually extends from 2 minutes to 5 minutes, the Young's modulus increases significantly to 80 GPa, and the hardness also increases synchronously to 2.3 GPa. However, the Young's modulus tends to be stable after the Si3N4 deposition time exceeds 3 minutes, with a relatively small change range. This result indicates that the introduction of Si3N4 significantly improves the mechanical properties of the composite structure, and its strengthening effect tends to saturate after the deposition time reaches a certain level. The strengthening effect of Si3N4 is mainly reflected in its high hardness and dense structure. In the composite material, Si3N4 forms a thin film with high hardness and good toughness, significantly improving the surface rigidity of the material and effectively hindering the expansion of dislocations. This strengthening effect enables the Young's modulus and hardness of the nanolayered composite material to continuously increase with the extension of the Si3N4 deposition time. In addition, the good combination of Si3N4 and the matrix material at the interface can form a strong constraint interface, thereby further improving the deformation resistance of the material. These characteristics indicate that the deposition of Si3N4 has an important optimization effect on the mechanical properties of the nanolayered composite material.

[0028] The protection scope of the present invention includes but is not limited to the above embodiments. The protection scope shall be subject to the claims. Any replacement, deformation, and improvement that are easily conceivable by those skilled in the art to the present technology fall within the protection scope of the present invention.

Claims

1. Cu-Si3N4-FeCoCrNiMn nanolayered composite material, characterized in that It includes multiple groups of layered composite units that are successively compounded and stacked. Each group of layered composite units is successively compounded and stacked by a Cu film, a Si3N4 film, and a FeCoCrNiMn film. The thickness of the Cu film is 30 - 100 nm, the thickness of the Si3N4 film is 5 - 15 nm, and the thickness of the FeCoCrNiMn film is 20 - 60 nm.

2. The Cu-Si3N4-FeCoCrNiMn nanolayered composite material according to claim 1, characterized in that: The thickness of the Cu film is 50 - 70 nm, the thickness of the Si3N4 film is 6 - 10 nm, and the thickness of the FeCoCrNiMn film is 30 - 50 nm.

3. The Cu-Si3N4-FeCoCrNiMn nanolayered composite material according to claim 1 or 2, characterized in that: The thickness of the Cu film is 60 nm, the thickness of the Si3N4 film is 8 nm, and the thickness of the FeCoCrNiMn film is 40 nm.

4. The Cu-Si3N4-FeCoCrNiMn nanolayered composite material according to claim 1, characterized in that: There are 6 - 10 groups of the described layered composite units.

5. The Cu-Si3N4-FeCoCrNiMn nanolayered composite material according to claim 1 or 4, characterized in that: There are 7 groups of the described layered composite units.

6. Preparation method of Cu-Si3N4-FeCoCrNiMn nanolayered composite material, characterized in that It includes the following specific steps: (1), Fix a Cu target, a FeCoCrNiMn target, and a Si3N4 target on the target head of a magnetron sputtering instrument respectively; (2) Reduce the pressure in the sputtering chamber of the magnetron sputtering instrument to 5×10 -4 Pa. Meanwhile, introduce argon gas as the sputtering medium, and perform pre-sputtering on the Cu target, FeCoCrNiMn target, and Si3N4 target respectively to remove the oxide layer or adsorbed impurities on the surface of the target materials; (3), First deposit a Cu thin film on the Si substrate, control the argon flow rate to be 50 sccm, the sputtering gas pressure to be 0.7 - 1.8 Pa, the power supply power to be 120 W, and the deposition time to be 5 minutes, so that the deposition thickness of the Cu thin film reaches 30 - 100 nm; (4), Then deposit a Si3N4 thin film on the Cu thin film, control the argon flow rate to be 50 sccm, the sputtering gas pressure to be 1.5 Pa, the power supply power to be 90 W, and the deposition time to be 2 - 5 minutes, so that the deposition thickness of the Si3N4 thin film reaches 5 - 15 nm; (5), Finally deposit a FeCoCrNiMn thin film on the Si3N4 thin film, control the argon flow rate to be 60 sccm, the sputtering gas pressure to be 1.3 - 2.3 Pa, the power supply power to be 120 W, and the deposition time to be 5 minutes, so that the deposition thickness of the FeCoCrNiMn thin film reaches 20 - 60 nm, thereby obtaining a group of layered composite units; (6), Then deposit a Cu thin film on the FeCoCrNiMn thin film of the layered composite unit, and repeat steps (3) - (5) 5 - 9 times in a cycle to obtain a Cu - Si3N4 - FeCoCrNiMn nanolayered composite material.

7. The preparation method of the Cu-Si3N4-FeCoCrNiMn nanolayered composite material according to claim 6, characterized in that: In the described step (1), the target purity of the Cu target is 99.9999%, the target purity of the FeCoCrNiMn target is 99.95%, and the target purity of the Si3N4 target is 99.9%.

8. The preparation method of the Cu-Si3N4-FeCoCrNiMn nanolayered composite material according to claim 6, characterized in that: In the described step (1), fix the Cu target and the FeCoCrNiMn target on the first permanent magnet target head and the strong magnet target head connected to the DC power supply respectively, and fix the Si3N4 target on the second permanent magnet target head connected to the RF power supply.

Images