A method for preparing a metal layered composite plate by using a contact reaction

By laying metal powder that can be eutectic-reactive in the metal plate to be composited in the metal layer composite plate, and heating after cold rolling and recombination, the metal powder and the base metal are contacted and reacted to form a high-hard intermetallic compound The pinned structure solves the problem of low interface bonding strength of metal layered composite plates in the prior art, and realizes the preparation of metal layered composite plates with high interface bonding strength.

CN114101681BActive Publication Date: 2025-02-07AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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Patent Information

Application Number
CN202111372595.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-11-18
Publication Date
2025-02-07
Estimated Expiration
2041-11-18

AI Technical Summary

Technical Problem

The prior art has problems such as high equipment requirements, complex process and low interface bonding strength when preparing metal layered composite panels, which affects the promotion and application of metal layered composite panels.

Method used

By laying metal powder that can react eutectic with the metal plate to be composited, and heating after cold rolling and recombination, the metal powder and the base metal are contacted and reacted to form a high-hard intermetallic compound Pin the structure to improve interface bonding strength.

Benefits of technology

It realizes the preparation of metal layered composite boards with high interface bonding strength. It has a wide range of materials, simple operation, and low equipment requirements. It is suitable for composite connections of two-layer or multi-layer boards.

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Abstract

The present invention discloses a method for preparing a metal layered composite plate by using a contact reaction, and belongs to the field of preparing metal-based composite materials. The method pre-places intermediate metal powder between metal plates to be composited, and then uses a special rolling mill to perform cold rolling composite, and then heats the intermediate metal to cause a contact reaction with the composite metal plate, and finally forms a composite interface in which a high-hardness intermetallic compound is pinned within the interface, thereby obtaining a metal layered composite plate with a high interface bonding strength. The present invention has low equipment requirements, can be used for composite connection of two or more layers of plates, has a wide range of material applications, is simple to operate, has low equipment requirements, and has great practical application value.
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Description

Technical Field

[0001] The invention belongs to the technical field of preparation of metal-based layered composite materials, and in particular provides a method for preparing a metal-based layered composite plate by utilizing contact reaction. Background Art

[0002] Metal composite plates are widely used in heat dissipation, communication, power and other industries because they have the physical, chemical, mechanical or price advantages of different metals. At present, the methods for preparing metal composite plates mainly include rolling composite, explosion composite, solid-liquid casting and rolling composite, etc. The rolling composite method is widely used in industrial production due to its simple process, high production efficiency and low cost. However, in order to improve the interface bonding strength, the required rolling deformation is generally large, and the equipment capacity is required to be high. The explosion composite method uses the huge energy generated by the explosion of explosives to instantly generate high temperature and high pressure between the bimetallic materials to achieve a firm bond between the welded metals. This method has a simple process and is not limited in product size, but it has a large restriction on the experimental site. The solid-liquid casting and rolling composite method is a new technology based on double-roll casting and rolling technology. It uses rotating rollers to quickly cool the liquid metal, so that the liquid metal forms a diffuse flow on the surface of the solid substrate, and then under the action of the rolling force, the liquid metal undergoes plastic deformation during the solidification process to prepare a bimetallic composite plate. The composite plate prepared by this method has high interface bonding strength, short process flow, and requires special equipment. In summary, the existing methods for preparing metal layered composite plates have problems such as high equipment requirements, complex processes, and low interface bonding strength, which greatly affect the promotion and application of metal layered composite plates.

[0003] Therefore, in view of the shortcomings of traditional process methods, a method for preparing metal layered composite plates using contact reaction is proposed, which is of great significance for preparing metal layered composite plates with high interface bonding strength. Summary of the invention

[0004] The purpose of the present invention is to propose a method for preparing a metal layered composite plate by using a contact reaction, by using a special cold rolling mill to cold-roll and composite the plate, and then heating the intermediate metal powder to contact and react with the base layer and the coating to achieve high-strength connection of the same / different metal plates.

[0005] The solution of the present invention is as follows: a layer of metal powder that can undergo eutectic reaction with the metal plates to be composited and generate brittle intermetallic compounds is spread between the metal plates to be composited, and then the combined metal plates are cold-rolled for composite, and finally heated, so that the metal powder and the base metal come into contact and react, thereby achieving effective connection between the plates to be composited.

[0006] A method for preparing a metal layered composite plate by using a contact reaction, wherein an intermediate layer of metal powder is pre-placed before cold rolling and composite to obtain a metal layered composite plate with high interface bonding strength, comprising the following steps:

[0007] Step 1: Lay the metal powder flat in a vacuum heating furnace for heating and heat preservation to remove the oxide layer on the powder surface. The metal powder should be laid flat during heating to prevent the metal powder from sticking during the heating process. Clean the base metal plate and the cladding metal plate to be composited at room temperature, and then grind the composite surface to make a hardened layer with dents appear on the composite surface. After grinding, the surface presents a bright metallic color, and the thickness of the hardened layer is 10 to 100 μm.

[0008] Step 2: Spread the metal powder on the surface of the base metal plate with a thickness of 0.1 mm to 1 mm, and then place the cladding metal plate on the base metal plate for overlapping and assembly;

[0009] Step 3: The green sheet is subjected to pressure sintering treatment, and the pressure is applied by counterweight or hydraulic device. Under the action of pressure and heat, the metal powders are bonded to each other and to the surfaces of the base metal plate and the cladding metal plate, which can effectively prevent the metal powders from being squeezed out of the composite interface under the action of roller extrusion during the subsequent cold rolling composite.

[0010] Step 4: The assembled blanks are sent to a special double-roll cold rolling mill with matching concave and convex surfaces for cold rolling and compounding, so that the surface hardened layers of the base metal plate and the cladding metal plate are cracked, and the intermediate layer metal powder is embedded in the surface hardened layer of the cold-rolled composite plate. Since the thickness of the cladding metal powder is small, not exceeding 1 mm, the metal powder is dispersed in the interface due to the increase in the length of the plate during cold rolling and compounding, and a composite interface in which the metal powder is pinned in the interface is obtained;

[0011] Step 5: The cold-rolled composite plate is heated and kept warm so that the metal powder undergoes a eutectic reaction with the surface of the base metal plate and the cladding metal plate. The hardness of the produced eutectic metal compound is higher than that of the base metal plate and the cladding metal plate, and finally a metal layered composite plate with a high interface bonding strength having an intermetallic compound pinning structure is formed.

[0012] Furthermore, the metal powder in step 1 is a single or multiple metal powders that can undergo eutectic reaction with the metal plate to be composited and generate high-hardness intermetallic compounds, and the metal powder particle size is ≤150 mesh, which can effectively prevent the metal powder from over-reacting with the metal plate and affecting the function of the metal layered composite plate.

[0013] Furthermore, the metal powder in step 1 is heated to 60% to 80% of its melting point, the heat preservation time is 30 to 60 minutes, and the vacuum degree during heating is 10 -2 Pa and below, when the metal powder is heated in the vacuum, the oxide film is decomposed and removed due to the low oxygen partial pressure and high temperature.

[0014] Furthermore, the base metal and the cladding metal are pure metal materials or alloy materials of the same or different types, and the width of the base metal and the cladding metal plates is ≥ 10 mm at the parallel ends of the special rolling rollers.

[0015] Furthermore, during the pressure sintering in step 3, the pressure is 1 to 5 MPa, the sintering temperature is 60% to 90% of the eutectic reaction temperature, and the holding time is 10 to 60 minutes. After the sintering is completed, it is required that the metal powders are bonded to each other, and between the metal powders and the base metal and the cladding metal. By controlling the pressure and eutectic reaction temperature during the above sintering, as well as the holding time, the bonding strength is controlled, and the stress during cold rolling composite deformation is avoided, so as to ensure that the metal powders can be separated and dispersed during cold rolling composite deformation of the plate.

[0016] Furthermore, the two ends of the rollers of the special double-roll cold rolling mill with special concave and convex matching are beveled, corrugated or other structural forms that can achieve edge sealing. The blanks should be fed in the center for cold rolling, and the blanks with a width of ≥5mm on both sides are located in the edge sealing area of ​​the rollers, which effectively prevents metal powder from overflowing from both sides during cold rolling.

[0017] Furthermore, in step 4, the cold rolling speed is less than 0.1 m / s and the cold rolling deformation is greater than the critical composite deformation. During the cold rolling composite process, the blank is uniformly elongated and deformed, cracks occur on the elongated and deformed surfaces of the base and cladding metal plates, and the metal powder is separated to form a composite interface in which the metal powder is dispersed and embedded in the metal plates.

[0018] Furthermore, in step 5, the heating temperature is from the eutectic reaction temperature to the melting temperature of the low melting point element, and the holding time is 15 to 60 minutes. After the heating is completed, the metal powder is required to eutectically react with the base metal and the coating metal to form a single layer of intermetallic compound. When a eutectic reaction occurs between certain metals, a variety of intermetallic compounds will be generated. When heated, one of the intermetallic compounds is generally generated first. As the holding time increases, the remaining types of intermetallic compounds are gradually generated between the above intermetallic compound and one of the metals. The intermetallic compound is a brittle phase, and the lattice constants between different intermetallic compounds are different, resulting in a very low bonding strength between the intermetallic compound layers. Therefore, when two or more layers of intermetallic compounds are generated, the bonding strength of the intermetallic compound pinning composite interface will be significantly reduced.

[0019] Furthermore, metal powder is added on top of the cladding metal plate in step 3, and a base metal plate is added, and the two are repeatedly stacked to form a composite blank, wherein the blank structure has 2 to 10 layers.

[0020] A metal layered composite plate is prepared by the above-mentioned method for preparing a metal layered composite plate by utilizing contact reaction.

[0021] Advantages and beneficial effects of the present invention

[0022] The advantages and beneficial effects of the present invention are as follows: the present invention proposes a process of pre-setting intermediate metal powder between the metal plates to be composited and then cold rolling + heating by a special rolling mill. During heating, the metal powder and the base metal undergo a contact eutectic reaction, forming a plurality of welding points and a high-hardness intermetallic compound pinning structure at the bonding interface. By controlling the process parameters of each link, the above-mentioned interface form will greatly improve the interface bonding strength of the composite plate, and can be used for composite connection of two or more layers of plates. The material has a wide range of applicability, is simple to operate, and has low equipment requirements. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 The process flow chart of the preparation of the metal layered composite plate with high interface bonding strength of the present invention is shown in FIG. 1 is a wire brush, 2 is the metal to be composited, 3 is the intermediate metal powder, 4 is the cold-rolled composite plate, and 5 is a heating furnace.

[0024] Figure 2 They are inclined concave-convex matching rollers, 1 is a concave roller, and 2 is a convex roller. DETAILED DESCRIPTION

[0025] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0026] The method for preparing a metal layered composite plate proposed in the present invention utilizes a process of pre-placing intermediate metal powder between the metal plates to be composited and then cold rolling and heat treatment by a special rolling mill to form multiple welding points and a high-hardness compound pinning structure at the bonding interface, thereby obtaining a metal layered composite plate with high interface bonding strength. Compared with the traditional cold rolling composite process, the required rolling phase change amount is lower, the equipment requirements are low, and the interface bonding strength is high.

[0027] Embodiment 1:

[0028] Preparation of 3A21 aluminum alloy / 6063 aluminum alloy composite plates.

[0029] Step 1: Place pure copper powder with a particle size of 150 mesh flat in a vacuum heating furnace for heating and insulation to remove the oxide film. The heating temperature is 1050°C, the insulation time is 30 minutes, and the vacuum degree during heating is less than 1.0×10 -3Pa. The surfaces of 3A21 aluminum alloy plates (length × width × thickness = 200 mm × 50 mm × 1 mm) and 6063 aluminum alloy plates (length × width × thickness = 200 mm × 50 mm × 3 mm) to be composited were cleaned using a handheld laser cleaning device to remove surface oil stains, and then a steel wire brush with a wire diameter of 0.3 mm was used to polish the surfaces to be composited to form a surface hardening layer with a thickness of 10 μm;

[0030] Step 2: Copper powder with a thickness of 0.2 mm is spread on the surface of the 6063 aluminum alloy plate to be composited, and then the 3A21 aluminum alloy plate is placed on top of the 6063 aluminum alloy plate to align and overlap the blank;

[0031] Step 3: Place the blank in a vacuum diffusion welding furnace for pressurized heating and sintering treatment, with a pressure of 1 MPa, a heating temperature of 400°C, and a holding time of 20 min. After heating, a blank with a relatively fixed position of the metal powder and the aluminum alloy plate is obtained;

[0032] Step 4: The superimposed billet is fed into a two-roller rolling mill with beveled rollers at both ends at a rolling speed of 0.05 m / s for single-pass cold rolling composite, with a cold rolling deformation of 45%, to obtain a cold rolling composite interface in which copper powder is embedded in the aluminum alloy plate;

[0033] Step 5: The cold-rolled composite plate is heated in an air atmosphere at a heating temperature of 500°C and a holding time of 30 minutes. The copper powder and the aluminum alloy plate undergo a eutectic reaction to generate an intermetallic compound CuAl2 having a harderness than that of the aluminum alloy plate. Finally, the plate is air-cooled to room temperature to obtain a 3A21 / 6063 aluminum alloy layered composite plate with a high interface bonding strength in the form of CuAl2 pinned in the aluminum alloy plate.

[0034] The 3A21 aluminum alloy / 6063 aluminum alloy composite plate obtained through the above steps has good corrosion resistance, an interface bonding strength of 82 MPa, and an interface bonding rate of 100%.

[0035] Embodiment 2:

[0036] Preparation of 1060 aluminum alloy / 6061 aluminum alloy / 1060 aluminum alloy composite plate.

[0037] Step 1: Place pure copper powder with a particle size of 200 mesh flat in a vacuum heating furnace for heating and heat preservation to remove the oxide film. The heating temperature is 1100°C, the insulation time is 20 minutes, and the vacuum degree during heating is less than 1.0×10 -3 Pa. The oil stains on the surfaces of the 1060 aluminum alloy plate (length × width × thickness = 500 mm × 50 mm × 1 mm) and the 6061 aluminum alloy plate (length × width × thickness = 500 mm × 50 mm × 3 mm) to be composited were cleaned with a degreasing agent, and then the surfaces to be composited were polished with a steel wire brush with a wire diameter of 0.5 mm to form a surface hardening layer with a thickness of 15 μm;

[0038] Step 2: Copper powder with a thickness of 0.1 mm is spread on the surface of the 1060 aluminum alloy plate to be composited, and then the 6061 aluminum alloy plate is placed on top of the 1060 aluminum alloy plate to align and overlap, and then copper powder with a thickness of 0.1 mm is spread on the surface of the 6061 aluminum alloy plate, and then the 1060 aluminum alloy plate is placed on top to align and overlap to form a 1060 / 6061 / 1060 assembly;

[0039] Step 3: Place the blank in a vacuum diffusion welding furnace for pressurized heating and sintering treatment, with a pressure of 1 MPa, a heating temperature of 350°C, and a holding time of 30 minutes, to obtain a blank in which the metal powder and the aluminum alloy plate are relatively fixed in position after heating;

[0040] Step 4: The stacked billet is fed into a two-roll rolling mill with corrugated rollers at both ends at a rolling speed of 0.02 m / s for single-pass cold rolling composite, with a cold rolling deformation of 50%, to obtain a cold rolling composite interface in which copper powder is embedded in the aluminum alloy plate;

[0041] Step 5: The cold-rolled composite plate is heated in an air atmosphere at a heating temperature of 500°C and a holding time of 30 minutes. The copper powder and the aluminum alloy plate undergo a eutectic reaction to generate an intermetallic compound CuAl2 having a harderness than that of the aluminum alloy plate. Finally, the plate is air-cooled to room temperature to obtain a 1060 / 6061 / 1060 aluminum alloy layered composite plate with a high interface bonding strength in the form of CuAl2 pinned in the aluminum alloy plate.

[0042] The 1060 / 6061 / 1060 aluminum alloy layered composite plate obtained through the above steps has excellent formability and corrosion resistance, an interface bonding strength of 75 MPa, and an interface bonding rate of 100%.

[0043] Embodiment 3:

[0044] Preparation of 304 stainless steel / Q235 carbon steel composite plates.

[0045] Step 1: Place titanium powder with a particle size of 150 mesh flat in a vacuum heating furnace for heating and heat preservation to remove the oxide film. The heating temperature is 1100°C and the insulation time is 60 minutes. The vacuum degree during heating is less than 1.0×10 -3 Pa. Use acetone to clean the oil stains on the surfaces of 304 stainless steel plates (length × width × thickness = 200 mm × 40 mm × 0.5 mm) and Q235 carbon steel plates (length × width × thickness = 200 mm × 40 mm × 2 mm) to be composited, and then use a wire brush with a wire diameter of 0.5 mm to polish the surfaces to be composited to form a surface hardening layer with a thickness of 10 μm;

[0046] Step 2: Cover the surface of the Q235 carbon steel plate to be composited with titanium powder with a thickness of 0.5 mm, and then align and overlap the 304 stainless steel plate;

[0047] Step 3: Place the blank into a vacuum diffusion welding furnace for pressurized heating and sintering treatment, with a pressure of 2 MPa, a heating temperature of 1000°C, and a holding time of 30 min. After heating, a blank with relatively fixed positions of metal powder and steel plate is obtained;

[0048] Step 4: The stacked billet is sent to a two-roll rolling mill with corrugated rollers at both ends at a rolling speed of 0.01 m / s for single-pass cold rolling and lamination, with a cold rolling deformation of 60%, to obtain a cold rolling composite interface in which titanium powder is embedded in the steel plate;

[0049] Step 5: The cold-rolled composite plate is heated in an air atmosphere at a heating temperature of 1200°C for a holding time of 30 minutes. The titanium powder and the steel plate undergo a eutectic reaction to generate an intermetallic compound FeTi having a harderness than that of the steel plate. Finally, the plate is air-cooled to room temperature to obtain a 304 stainless steel / Q235 carbon steel layered composite plate with a high interface bonding strength in the form of FeTi pinned in the steel plate.

[0050] The 304 stainless steel / Q235 carbon steel layered composite plate obtained through the above steps has excellent formability and corrosion resistance, an interface bonding strength of 102 MPa, and an interface bonding rate of 100%.

[0051] The above is only a specific embodiment of the present invention, and the present invention is described in detail. The unexplained part is a conventional technology. However, the protection scope of the present invention is not limited to this. Any changes or substitutions that can be easily thought of by any technician familiar with the technical field within the technical scope disclosed by the present invention should be included in the protection scope of the present invention. The protection scope of the present invention shall be based on the protection scope of the claims.

Claims

1. A method for preparing a metal layered composite plate by using a contact reaction, wherein a metal layered composite plate with high interface bonding strength is obtained by pre-arranging an intermediate layer of metal powder before cold rolling and laminating, characterized in that: For preparing 3A21 aluminum alloy / 6063 aluminum alloy composite plate, 1060 aluminum alloy / 6061 aluminum alloy / 1060 aluminum alloy composite plate, or 304 stainless steel / Q235 carbon steel composite plate, the method comprises the following steps: Step 1: Place the metal powder in a vacuum heating furnace for heating and heat preservation to remove the oxide film on the powder surface. During heating, the metal powder is laid flat. The base metal plate and the cladding metal plate to be composited are cleaned at room temperature. Then, the composite surface is polished to form a hardened layer with dents. After polishing, the surface presents a bright metallic color, and the thickness of the formed hardened layer is 10 to 100 μm. Step 2: Spread the metal powder on the surface of the base metal plate with a thickness of 0.1 mm to 1 mm, and then place the cladding metal plate on the base metal plate for overlapping and assembly; Step 3: The green sheet is subjected to pressure sintering treatment, and the pressure is applied by counterweight or hydraulic device, so that the metal powders are bonded to each other and to the surface of the base layer and the cladding metal plate; during the pressure sintering, the pressure is 1-5 MPa, the sintering temperature is 60%-90% of the eutectic reaction temperature, and the holding time is 10-60 minutes; Step 4: The assembled blanks are sent to a special double-roll cold rolling mill with matching concave and convex surfaces for cold rolling and compounding, so that the surface hardened layers of the base metal plate and the cladding metal plate are cracked, and the intermediate layer metal powder is embedded in the interface hardened layer of the cold-rolled composite plate; Step 5: heating and keeping the cold-rolled composite plate warm, so that the metal powder reacts with the surface of the base metal plate and the cladding metal plate to form a eutectic reaction, and the resulting intermetallic compound has a higher hardness than the base metal plate and the cladding metal plate, thereby forming a metal layered composite plate with high interface bonding strength; The metal powder in step 1 is a single or multiple metal powders that can undergo eutectic reaction with the metal sheet to be composited and generate high-hardness intermetallic compounds, and the particle size of the metal powder is ≤150 mesh; The metal powder is heated to 60% to 80% of its melting point in step 1, and the holding time is 30 to 60 minutes. The vacuum degree during heating is 10 -2 Pa and below; When preparing 3A21 aluminum alloy / 6063 aluminum alloy composite plate, step 1 is: placing pure copper powder with a particle size of 150 mesh flat in a vacuum heating furnace for heating and heat preservation to remove the oxide film, the heating temperature is 1050°C, the heat preservation time is 30 minutes, and the vacuum degree during heating is less than 1.0×10 -3 Pa; Use a handheld laser cleaning device to clean the surfaces of the 3A21 aluminum alloy plate and the 6063 aluminum alloy plate to be composited to remove surface oil stains, and then use a wire brush with a wire diameter of 0.3 mm to polish the surfaces to be composited to form a surface hardening layer with a thickness of 10 μm; When preparing 1060 aluminum alloy / 6061 aluminum alloy / 1060 aluminum alloy composite plate, step 1 is: placing pure copper powder with a particle size of 200 mesh flat in a vacuum heating furnace for heating and heat preservation to remove the oxide film, the heating temperature is 1100°C, the heat preservation time is 20 minutes, and the vacuum degree during heating is less than 1.0×10 -3 Pa; using a degreasing agent to clean the oil stains on the surfaces of the 1060 aluminum alloy plate and the 6061 aluminum alloy plate to be composited, and then using a wire brush with a wire diameter of 0.5 mm to polish the surfaces to be composited to form a surface hardening layer with a thickness of 15 μm; When preparing 304 stainless steel / Q235 carbon steel composite plate, step 1 is: lay titanium powder with a particle size of 150 mesh flat and place it in a vacuum heating furnace for heating and insulation to remove the oxide film. The heating temperature is 1100°C, the insulation time is 60 minutes, and the vacuum degree during heating is less than 1.0×10 -3 Pa; acetone was used to clean the oil stains on the surfaces of the 304 stainless steel plate and the Q235 carbon steel plate to be composited, and then a wire brush with a wire diameter of 0.5 mm was used to polish the surfaces to be composited to form a surface hardening layer with a thickness of 10 μm.

2. A method for preparing a metal layered composite plate by contact reaction according to claim 1, characterized in that: The base metal and cladding metal are pure metal materials or alloy materials of the same or different types, and the width of the base metal plate and the cladding metal plate is ≥ 10mm at the parallel end of the special rolling roller.

3. A method for preparing a metal layered composite plate by contact reaction according to claim 1, characterized in that: The two end heads of the rollers of the special double-roller cold rolling mill with special concave-convex matching are bevel-shaped, corrugated-shaped or other structures that can achieve edge sealing.

4. A method for preparing a metal layered composite plate by contact reaction according to claim 3, characterized in that: In step 4, the cold rolling speed is less than 0.1 m / s and the cold rolling deformation is greater than the critical composite deformation.

5. The method for preparing a metal layered composite plate by contact reaction according to claim 1, characterized in that: In step 5, the heating temperature is from the eutectic reaction temperature to the melting temperature of the low melting point element, and the holding time is 15 to 60 minutes. After the heating is completed, the metal powder reacts with the base metal and the cladding metal to form a single-layer intermetallic compound.

6. A method for preparing a metal layered composite plate by contact reaction according to claim 5, characterized in that: In step 3, metal powder is added on top of the cladding metal plate, and a base metal plate is added, and the two are repeatedly stacked to form a composite blank, wherein the blank structure has 2 to 10 layers.

Citation Information

Patent Citations

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