CN116372344A - Hot isostatic pressure diffusion connection preparation method of Mg-Ta layered composite metal plate - Google Patents
Hot isostatic pressure diffusion connection preparation method of Mg-Ta layered composite metal plate Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 53
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- 229910019400 Mg—Li Inorganic materials 0.000 claims abstract description 48
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/023—Thermo-compression bonding
- B23K20/026—Thermo-compression bonding with diffusion of soldering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/26—Auxiliary equipment
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Abstract
The invention relates to a hot isostatic pressing diffusion connection preparation method of an Mg-Ta layered composite metal plate, and belongs to the technical field of hot isostatic pressing. The method solves the technical problems that the production efficiency of the Mg-Ta layered composite metal plate preparation process in the prior art is low, and the interface bonding capability is poor when the composite plate of Ta and dissimilar metals is prepared by adopting hot isostatic pressure diffusion connection. According to the preparation method, surface roughening and Al film plating are firstly carried out on a plurality of pure Ta plates, then a plurality of biphase Mg-Li alloy plates and a plurality of pure Ta plates are alternately stacked in sequence, and after being packed into a sheath for fixation, vacuumizing and hot isostatic pressing are carried out, so that the Mg-Ta layered composite metal plate is obtained. The preparation method is high in efficiency, suitable for preparing large-area composite metal plates, high in strength, strong in size and quality stability, and particularly suitable for processing and manufacturing the radiation-resistant light layered composite material for the shielding structure of the deep space detector.
Description
Technical Field
The invention belongs to the technical field of hot isostatic pressing, and particularly relates to a hot isostatic pressing diffusion connection preparation method of an Mg-Ta layered composite metal plate.
Background
The satellite cuisine of cuisine is considered to be the most likely existence of life, and exploration of cuisine has important significance in seeking life outside the earth. However, two technical difficulties are faced in order to successfully detect the wooden star. Firstly, the problem of high-density high-energy particle radiation of a strong surface magnetic field of the wooden star and a circular wooden star orbit, and secondly, the problem of energy sources caused by the remote distance of the wooden star. This places a dual requirement on the high energy particle irradiation resistance and light weight of the instrumentation of the detector. The upgrading of light weight and the substantial weight reduction based on the existing structural design, materials and process technology are one of the important development directions of deep space exploration technology research in China (Optimization Design of Radiation Vault in Jupiter Orbiting Mission [ J ], J.Z.Wang, J.N.Ma, J.W.Qiu, D.Tian, A.W.Zhu, Q.X. Zhang, A.S. Zhou.IEEE Transactions on Nuclear Science, (66) 2019, 2179-2187). Wherein, the composite of the heavy metal radiation-resistant materials Ta, nb and the like and the light structural metal material Mg is expected to relieve two technical problems of irradiation and energy faced by the wooden star detector. Analysis and calculation research on an anti-radiation material system of the wooden star detector structure show that the Mg-Ta layered composite board can effectively reduce the weight by about 45.1 percent on the premise of having the same anti-radiation effect as a heavy metal material, and has great potential in the development of deep space detection technology. However, because Mg and Ta metallurgies are not compatible, there are great differences in physical and chemical properties and metallurgical properties such as the melting point of the two metals (the melting point of Ta is 2996 ℃ and the melting point of Mg is 650 ℃), the lattice type (Ta is BCC and Mg is HCP), the linear expansion coefficient, and the like, so Mg-Ta connection is difficult, and few reports about the Mg-Ta layered composite board preparation process at home and abroad exist.
The Chinese patent with publication number of CN113733685A reports a light high-strength Mg-Al-Ta composite metal plate and a rolling forming method thereof, although the processing and the preparation of the Mg-Ta layered composite plate can be realized, the process of the composite metal plate involves respectively carrying out heat preservation treatment at different temperatures on the Mg plate and the pure Ta plate, then stacking and fixing the plates, the temperature change of the stacked plates is difficult to effectively control before rolling deformation, and the production efficiency is low; the Chinese patent with publication number of CN113352708A reports a light high-strength Mg-Ta composite metal plate and a room-temperature rolling forming method thereof, and the preparation method avoids the problems of plate oxidation and energy consumption possibly brought by middle-high temperature rolling, but ensures the smooth running of rolling deformation in order to effectively reduce the residual stress among different metal plates, needs to introduce low-temperature recovery annealing and high-temperature diffusion annealing among rolling passes, needs to perform rolling deformation of multiple passes, and has low production efficiency; the Chinese patent with publication number of CN112742870A reports a preparation method of a shielding type magnesium-tantalum multilayer composite board, although the processing and preparation of Mg-Ta layered composite boards can be realized, the technology of the shielding type magnesium-tantalum multilayer composite board involves the adoption of vacuum high-temperature rolling to avoid the oxidation problem of boards, and has high requirements on rolling equipment and rolling environment and low production efficiency.
Most of the preparation methods adopted in the patent are multi-pass medium-high temperature rolling processing and annealing heat treatment, and reports on preparing Mg-Ta layered composite plates through hot isostatic pressing diffusion connection are still fresh at present. Compared with the rolling process, the hot isostatic pressing technology has the characteristics of high production efficiency and high process stability, and can be used for obtaining large-area high-strength solid phase connection. The hot isostatic pressing technology has been shown to be applicable to large-area high-strength solid phase connection of Ta and Cu, ta and Al and other dissimilar metals (solid phase connection structure and performance research of high-purity metal tantalum and copper alloy [ D ], qian Gongbing, harbin university of industry). Chinese patent publication No. CN101733544a reports a diffusion welding method for obtaining tantalum and copper, aluminum, titanium dissimilar metals using hot isostatic pressing.
However, solid phase connection studies of Ta and a dissimilar metal show that Ta and a dissimilar metal are difficult to be combined, and the main reason is that Ta is extremely easy to form a dense oxide film and has a remarkable self-repairing capability.
In addition, in the technique of compositing Ta with a dissimilar metal, there is no method for improving the interfacial bonding ability between Ta and the dissimilar metal from the viewpoints of surface roughness and surface quality.
Disclosure of Invention
The invention aims to solve the technical problem of low production efficiency of a Mg-Ta layered composite metal plate preparation process in the prior art.
The second purpose of the invention is to solve the technical problem that the interface bonding capability is poor in the prior art that the composite board of Ta and dissimilar metals is prepared by adopting hot isostatic pressing diffusion connection.
The technical scheme adopted by the invention for achieving the purpose is as follows.
The invention provides a hot isostatic pressing diffusion connection preparation method of an Mg-Ta layered composite metal plate, which comprises the following steps:
firstly, polishing surfaces of a plurality of biphase Mg-Li alloy plates and a plurality of pure Ta plates, cleaning and vacuum drying;
step two, carrying out surface roughening, acid washing, cleaning and vacuum drying on the cleaned pure Ta plates obtained in the step one;
plating Al films on the surfaces of the pure Ta plates subjected to the vacuum drying in the step two;
step four, cleaning the cleaned two-phase Mg-Li alloy plates obtained in the step one and the cleaned pure Ta plates coated with the Al film obtained in the step three, sequentially and alternately stacking after vacuum drying, loading into a sheath for fixation, and vacuumizing to obtain a to-be-pressed piece;
and fifthly, carrying out hot isostatic pressing on the to-be-pressed piece, and removing the sheath to obtain the Mg-Ta layered composite metal plate.
Preferably, in the first step, an angle grinder is used for polishing the surfaces of the Mg-Li alloy sheet and the pure Ta sheet.
Preferably, in the first step, the cleaning is chemical cleaning.
Preferably, in the first step, the temperature of the vacuum drying is 100-150 ℃.
Preferably, in the second step, the surface Mao Huawei of the pure Ta plate is formed by machining threads or bosses on the surface of the pure Ta plate. More preferably, in the second step, the surface roughening process is performed on the pure Ta plate by turning.
Preferably, in the second step, the pickling is performed for 20-40 seconds by using Ta pickling solution.
Preferably, in the second step, the cleaning is performed by washing with deionized water and then ultrasonic cleaning with IPA.
Preferably, in the second step, the temperature of vacuum drying is 100-150 ℃.
Preferably, in the third step, the Al film is coated by magnetron sputtering at 18-28deg.C with a magnetron sputtering power of 250-350W, a chamber pressure of 3.5-4.0X10 Torr, a substrate rotation speed of 5-8r/min, and a sputtering rate of 30-40nm/min.
Preferably, before the third step, the pure Al target material adopted by the Al film plating is subjected to magnetron sputtering to remove surface oxides.
Preferably, in the fourth step, the cleaning is chemical cleaning.
Preferably, in the fourth step, the temperature of the vacuum drying is 100-150 ℃.
Preferably, in the fourth step, after being stacked alternately in turn, the upper surface is a dual-phase Mg-Li alloy plate, and the lower surface is a pure Ta plate.
Preferably, in the fifth step, the hot isostatic pressing is performed under nitrogen protection, the pressure is 100-120MPa, the temperature is (0.6-0.8) x 650 ℃ of the Mg melting point, and the time is more than 3-5 h.
The principle of the invention is as follows: according to the preparation method for the Mg-Ta layered composite metal plate by hot isostatic pressing diffusion connection, the Mg-Li alloy plate and the pure Ta plate with roughened surfaces and plated with the Al film are sequentially stacked and fixed according to a set sequence, the Mg-Li alloy plate and the pure Ta plate are composited by vacuum hot isostatic pressing at the temperature of (0.6-0.8) Tm (Mg), and the problem that Mg and Ta are difficult to cooperatively and greatly plastically deform in a rolling process is avoided by utilizing the vacuum hot isostatic pressing. In the process, the surface of the pure Ta plate is roughened, and surface burrs are forced to be extruded into the Mg-Li alloy plate by pressure in the vacuum hot isostatic pressing process, so that dissimilar metal atoms on two sides of a connecting interface of the Mg-Li alloy plate are subjected to interdiffusion reaction, and a very good solid phase connecting effect between the Mg-Li alloy plate and the pure Ta plate is realized. The magnetron sputtering surface is used for plating the Al film, so that on one hand, the surface oxidation of a pure Ta plate is avoided, and on the other hand, the pure Ta plate and the Mg-Li alloy plate are bonded as an intermediate layer, so that the diffusion connection of two mutually insoluble systems is improved. And carrying out vacuum hot isostatic pressing on the pure Ta plate and the Mg-Li alloy plate subjected to surface roughening and Al film plating, wherein the vacuum hot isostatic pressing ensures that the pure Ta plate and the Mg-Li alloy plate are macroscopically not deformed, avoids plastic instability and residual stress among deformed plates in a rolling process, and can realize effective metallurgical bonding in the vacuum hot isostatic pressing heat preservation process after mechanical bonding is realized by using the surface roughening. The whole process is carried out under the vacuum condition, so that the generation of a surface oxide layer is avoided, and the surface bonding strength is ensured; meanwhile, the method is simple in process and comprises magnetron sputtering and hot isostatic pressing, so that the preparation efficiency of the Mg-Ta layered composite metal plate is high, the method is suitable for preparing the composite metal plate, and the prepared Mg-Ta layered composite metal plate is high in strength and high in dimensional and quality stability.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the preparation method of the Mg-Ta layered composite metal plate by hot isostatic pressing diffusion connection, the light Mg-Li alloy plate with two phases is adopted to replace the traditional AZ series Mg alloy plate, and the light Mg-Li alloy plate and the pure Ta plate with roughened surfaces and plated with Al films are subjected to medium-temperature stack hot isostatic pressing, so that the quality of the plate can be obviously reduced, and the space carrying capacity can be improved; meanwhile, the BCC crystal structure of the Li phase in the Mg-Li alloy plate and the Ta phase in the pure Ta plate is beneficial to the atomic diffusion of the Mg-Li alloy plate and the pure Ta plate, and the interface bonding strength is improved.
2. According to the preparation method for the Mg-Ta layered composite metal plate by hot isostatic pressing diffusion connection, the hot isostatic pressing technology is adopted to carry out solid-phase diffusion connection on Mg and Ta, compared with the Mg-Ta layered composite metal plate prepared by the traditional multi-pass complex process such as rolling, multi-pass intermediate annealing and the like, the preparation method has the remarkable advantages of short production period, less working procedures and low energy consumption, and the size and quality stability of the Mg-Ta layered composite metal plate prepared by hot isostatic pressing are high due to the fact that the technological parameters in the hot isostatic pressing process are few and more controllable.
3. According to the preparation method for the hot isostatic pressing diffusion connection of the Mg-Ta layered composite metal plate, the pure Ta plate is subjected to surface roughening, so that the problem of mechanical combination caused by difficulty in coordination of plasticity, easiness in generation of residual stress and the like of Mg and Ta greatly different dissimilar metals is effectively solved.
4. According to the preparation method for the hot isostatic pressing diffusion connection of the Mg-Ta layered composite metal plate, disclosed by the invention, the magnetron sputtering process method is adopted to carry out low-temperature Al film plating on the pure Ta plate, so that the problem of surface oxidation of each metal layer when the composite intermediate Al layer is adopted in middle-high temperature hot pressing or rolling is avoided. And the magnetron sputtering Al film has low cost, is not limited by the type and shape of the substrate, and has high deposition rate and low deposition temperature, so that the Al film has few impurities and high quality. The Al film coated on the Ta surface effectively solves the problems of surface oxidation and difficult metallurgical bonding with Mg of pure Ta plates in the hot isostatic pressing solid phase connection process.
5. The preparation method of the Mg-Ta layered composite metal plate by hot isostatic pressing diffusion connection is particularly suitable for processing and manufacturing the radiation-resistant light layered composite material for the shielding structure of the deep space detector.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that it is possible for a person skilled in the art to obtain different kinds of drawings from these drawings without inventive effort.
FIG. 1 is a flow chart of a process for preparing a HIP Mg-Ta layered composite metal sheet of the present invention.
FIG. 2 is a schematic diagram of the structure of a HIP'd Mg-Ta layered composite metal sheet of the present invention;
in the figure, 1, mg-Li alloy plate, 2, pure Ta plate, 2-1, surface roughening, 2-2 and Al film.
FIG. 3 is a scanning electron micrograph of an interface of a Mg-Ta layered composite metal sheet of example 1 of the invention.
FIG. 4 is a scanning electron micrograph of an interface of a Mg-Ta layered composite metal sheet of example 2 of the invention.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the invention are described below, but it is to be understood that these descriptions are merely intended to illustrate further features and advantages of the invention, and are not limiting of the claims of the invention.
The invention relates to a preparation method of a Mg-Ta layered composite metal plate by hot isostatic pressing diffusion connection, which comprises the following steps:
firstly, polishing and cleaning the surfaces of a plurality of biphase Mg-Li alloy plates 1 and a plurality of pure Ta plates 2, removing surface oxide layers and impurities, and drying in vacuum;
step two, carrying out surface roughening 2-1 on the cleaned pure Ta plates 2 obtained in the step one, carrying out acid washing, cleaning and vacuum drying;
plating Al films 2-2 on the surfaces of the pure Ta plates 2 after the vacuum drying in the step two;
step four, cleaning the cleaned two-phase Mg-Li alloy plates 1 obtained in the step one and the pure Ta plates 2 plated with the Al films 2-2 obtained in the step three, removing surface oxide layers and impurities, carrying out vacuum drying, sequentially and alternately stacking, loading into a sheath for fixation, welding, and vacuumizing to obtain a to-be-pressed piece;
and fifthly, carrying out hot isostatic pressing on the to-be-pressed piece, mechanically meshing and metallurgically combining the Mg-Li alloy plate 1, the pure Ta plate 2 and the Al-plated film 2-2, and mechanically processing to remove the sheath, thereby obtaining the Mg-Ta layered composite metal plate.
In the technical scheme, the Mg-Li alloy plate 1 and the pure Ta plate 2 can be obtained by commercial purchase and are subjected to stress relief annealing heat treatment. Wherein the Mg-Li alloy sheet material 1 has a dual-phase structure, namely an alpha+beta phase, the Li phase in the Mg-Li alloy sheet material and the Ta in the pure Ta sheet material have the same BCC crystal structure, and the Mg-Li alloy sheet material 1 preferably adopts LA86M. The initial thickness of the Mg-Li alloy sheet 1 and the pure Ta sheet 2 is typically 2-3mm. The number of the plurality of the catalyst is not particularly limited, and the number of the catalyst can be more than 1 and can be determined according to actual needs.
In the above technical scheme, in the first step, the mg—li alloy plate 1 and the pure Ta plate 2 are preferably surface polished by an angle grinder. It should be noted that other surface finishing processes known to those skilled in the art are suitable for use with the present invention.
In the above technical solution, in the first step, the cleaning is chemical cleaning, and the chemical cleaning is not particularly limited, and the cleaning may be performed in a manner well known to those skilled in the art, so long as the effect of removing the surface oxide layer and the impurities is achieved. H is generally used 2 SO 4 ：HF：HNO 3 Surface treatment was performed with =3:2:1 mixed acid.
In the above technical scheme, in the first step, the temperature of vacuum drying is 100-150 ℃, and the drying equipment is not particularly limited, and is usually a vacuum drying oven.
In the above technical solution, in the second step, the surface roughening 2-1 of the pure Ta plate 2 is preferably performed by machining a thread or a boss on the surface of the pure Ta plate 2, where the size of the thread or boss is determined according to actual needs. For example, the thread pitch is 0.4-0.5mm, the thread depth is 0.1-0.2mm, and the thread angle is 97-100 degrees; the height of the boss is 0.4-0.5mm, the depth of the boss is 0.1-0.3mm, and the angle of the boss is 90 degrees. The process typically employed to roughen the surface 2-1 of a pure Ta plate 2 is turning. However, it should be noted that other processing methods known to those skilled in the art are also suitable for the present invention.
In the second step, the pickling is carried out for 20-40s, preferably 30s, of Ta pickling solution. The Ta pickling is not particularly limited as long as it has an effect of completely exposing the fresh metal surface.
In the second step, the washing is carried out by washing with deionized water and then ultrasonic washing with IPA. However, other cleaning known to those skilled in the art is also applicable to the present invention, as long as the acid for pickling is removed.
In the above technical scheme, in the second step, the temperature of vacuum drying is 100-150 ℃, and the drying equipment is not particularly limited, and is usually a vacuum drying oven.
In the third step, the process adopted by the Al film 2-2 is magnetron sputtering, preferably direct current magnetron sputtering, and the pure Ta plate 2 has fine, uniform and compact aluminum particles, almost no defects such as white agglomerates and holes on the surface, and good adhesiveness. The preferable process conditions of the magnetron sputtering are as follows: the magnetron sputtering temperature is 18-28 ℃, the magnetron sputtering power is 250-350W, the chamber pressure is 3.5-4.0x10 Torr, the substrate rotating speed is 5-8r/min, and the sputtering rate is 30-40nm/min; more preferably, the magnetron sputtering power is 300W, the chamber pressure is 3.7X10 Torr, the substrate rotation speed is 6r/min, and the sputtering rate is 36nm/min. Preferably, before the third step, the pure Al target material adopted by the Al film 2-2 is subjected to magnetron sputtering to remove surface oxides. The Al film 2-2 prevents the pure Ta plate 2 from forming a self-repairing oxide film and improves the interfacial bonding capability of the Mg-Li alloy plate 1 and the pure Ta plate 2.
In the above technical scheme, in the fourth step, the cleaning is chemical cleaning, and the cleaning is not particularly limited, and the cleaning can be performed in a manner well known to those skilled in the art, so long as the effect of removing the surface oxide layer and the impurities is achieved. Typically a chemical acid wash.
In the above technical scheme, in the fourth step, the temperature of vacuum drying is 100-150 ℃, and the drying equipment is not particularly limited, and is usually a vacuum drying oven.
In the above technical solution, after the stacking is sequentially and alternately performed in the fourth step, there is no special limitation on the uppermost layer and the lowermost layer, and the upper surface is usually a dual-phase Mg-Li alloy plate 1, and the lower surface is usually a pure Ta plate 2. However, the number of the Mg-Li alloy plate 1 and the pure Ta plate 2 is not particularly limited, and may be equal or unequal, and the thickness of the Mg-Ta layered composite metal plate prepared according to actual needs may be set, and the thicknesses of the single plates of the Mg-Li alloy plate 1 and the pure Ta plate 2 are usually 2mm, but the invention is not limited thereto. The upper and lower surfaces of the Mg-Ta layered composite metal plate are not particularly limited, and may be both a dual-phase Mg-Li alloy plate 1, a pure Ta plate 2, or one of the dual-phase Mg-Li alloy plates 1 and the other pure Ta plate 2.
In the technical scheme, in the step five, the hot isostatic pressing process condition is that the pressure is 100-120MPa, the temperature is (0.6-0.8) multiplied by 650 ℃ of the Mg melting point, and the time is more than 3-5 h. Preferably, the pressure is 100MPa, the temperature is 0.6-0.8 of the melting point of Mg, and the time is more than 5 hours. The gas is preferably nitrogen.
In the above technical solution, in the fifth step, the sheath is preferably a stainless steel sheath.
The terms used in the present invention generally have meanings commonly understood by those of ordinary skill in the art unless otherwise indicated. In order to enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be described in further detail with reference to examples.
In the following examples, various processes and methods, which are not described in detail, are conventional methods well known in the art. Materials, reagents, devices, instruments, equipment and the like used in the examples described below are commercially available unless otherwise specified.
The invention is further illustrated below with reference to examples.
Example 1
The hot isostatic pressing diffusion connection preparation method of the Mg-Ta layered composite metal plate comprises the following steps:
step one, three Mg-Li alloy plates 1 (LA 103M, initial thickness 2-3mm, area 1000 mm) 2 Conforms to GB/T5153-2016, in annealed state) and three pure Ta plates 2 (initial thickness 2-3mm, purity 99.95% and area 1000 mm) 2 Annealed) is polished by an angle grinder for 3-5min, surface pollution and oxide layer are removed, and the glass is cleaned and dried in vacuum.
And step two, turning threads on the surface of the pure Ta plate 2 processed in the step one, wherein the thread pitch is 0.45mm, the thread depth is 0.2mm, the thread angle is 97 degrees, immersing into a Ta pickling solution for chemical cleaning for 30s, removing surface oxides and impurities, and drying in vacuum.
Step three, using direct current magnetron sputtering equipment to make pure Al target material (purity is above 99.5%, area is 1000 mm) 2 According with GB/T3880-2006, annealing state) to remove surface oxide by pre-sputtering, then plating Al film 2-2 on the surface of pure Ta plate 2 at low temperature (20 ℃) by using direct current magnetron sputtering equipment, and performing magnetic sputteringThe sputtering power is controlled to be 300W, the chamber pressure is 3.7X10 Torr, the substrate rotating speed is 6r/min, and the sputtering rate is 36nm/min, so that the surface of the pure Ta plate 2 is covered with a uniform and compact Al film 2-2.
And fourthly, chemically cleaning the Mg-Li alloy plate 1 and the pure Ta plate 2 coated with the Al film 2-2 obtained in the first step again to remove surface oxides and impurities, sequentially and alternately stacking the Mg-Li alloy plate 1 and the pure Ta plate 2 coated with the Al film 2-2 (Mg-Ta-Mg-Ta), loading the materials into a stainless steel sleeve container for fixation as shown in fig. 2, and vacuumizing the stainless steel sleeve after welding.
Putting the stainless steel sleeve into a hot isostatic pressing device, wherein hot isostatic pressing gas is nitrogen, the pressure is 100MPa, the hot isostatic pressing temperature is 350 ℃, after the heat preservation time is 5 hours, the threads of the pure Ta plate 2 are completely extruded into the Mg-Li alloy plate 1, the Mg-Ta mechanical combination is good, and the atomic diffusion of each layer of Mg, al and Ta is realized under the action of temperature and pressure, wherein the beta phase of the Al coating 2-2 and the Mg-Li alloy plate 1 provides an effective diffusion channel for Mg and Ta, and the diffusion connection of two insoluble metals of the Mg-Li alloy plate 1 and the pure Ta plate 2 is promoted.
And step six, removing the stainless steel sheath by utilizing machining to obtain the Mg-Ta layered composite metal plate with high interface bonding strength and no residual stress.
Example 2
The hot isostatic pressing diffusion connection preparation method of the Mg-Ta layered composite metal plate comprises the following steps:
step one, two Mg-Li alloy sheets 1 (LA 86M, initial thickness 3mm, area 1000 mm) 2 The alloy meets GB/T5153-L2016 in an annealed state) and two pure Ta plates 2 (with an initial thickness of 2mm, a purity of 99.95 percent and an area of 1000mm 2 Annealed) is polished by an angle grinder for 3-5min, surface pollution and oxide layer are removed, and the glass is cleaned and dried in vacuum.
Turning the surface of the pure Ta plate 2 processed in the step one to form a boss with the height of 0.45mm and the depth of 0.2mm and the angle of 90 degrees, immersing the boss into a Ta pickling solution to perform chemical cleaning for 30s, removing surface oxides and impurities, and performing vacuum drying.
Step three, utilizing direct current magnetic controlSputtering equipment for pure Al target material (purity is above 99.5%, area is 1000 mm) 2 According with GB/T3880-2006, annealing state), performing pre-sputtering to remove surface oxide, and then plating an Al film 2-2 on the surface of a pure Ta plate 2 at a low temperature (20 ℃) by using a direct current magnetron sputtering device, wherein the magnetron sputtering power is 320W, the chamber pressure is 3.7X10 Torr, the substrate rotating speed is 6r/min, and the sputtering rate is 36nm/min, so that the Ta surface is covered with a uniform and compact Al film 2-2.
And fourthly, chemically cleaning the Mg-Li alloy plate 1 and the pure Ta plate 2 coated with the Al film 2-2 obtained in the first step again to remove surface oxides and impurities, sequentially alternately stacking the Mg-Li alloy plate 1 and the pure Ta plate 2 coated with the Al film 2-2 (Mg-Ta-Mg-Ta), loading into a stainless steel sleeve container for fixation, and vacuumizing the stainless steel sleeve after welding.
Putting the stainless steel sleeve into a hot isostatic pressing device, wherein hot isostatic pressing gas is nitrogen, the pressure is 150MPa, the hot isostatic pressing temperature is 400 ℃, after the heat preservation time is 8 hours, the pure Ta plate 2 is completely extruded into the Mg-Li alloy plate 1 by threads, the Mg-Ta is well mechanically combined, and the atomic diffusion of each layer of Mg, al and Ta is realized under the action of temperature and pressure, wherein an effective diffusion channel is provided for Mg and Ta by the beta phase of the Al film 2-2 and the Mg-Li alloy plate 1, and the diffusion connection of two insoluble metals of the Mg-Li alloy plate 1 and the pure Ta plate 2 is promoted.
And step six, removing the stainless steel sheath by utilizing machining to obtain the Mg-Ta layered composite metal plate with high interface bonding strength and no residual stress.
Comparative example 1
The preparation method of the Mg-Ta layered composite metal sheet of this comparative example was the same as that of example 1, except that the pure Ta sheet 2 was not subjected to surface roughening 2-1.
Comparative example 2
The preparation method of the Mg-Ta layered composite metal sheet of the present comparative example is the same as that of example 1, except that the pure Ta sheet 2 is not subjected to the Al film plating 2-2 treatment, and the Al target is directly involved in stacking as an intermediate layer in the order Mg-Al-Ta-Mg-Al-Ta.
Comparative example 3
The preparation method of the Mg-Ta layered composite metal sheet of this comparative example is the same as that of example 1, except that the pure Ta sheet 2 was not subjected to the Al plating film 2-2.
Comparative example 4
The preparation method of the Mg-Ta layered composite metal sheet of the present comparative example is the same as that of example 1, except that the Mg-Li alloy sheet 1 is an HCP single-phase Mg-3Li alloy sheet.
The Mg-Ta layered composite metal sheets prepared in examples 1-2 and comparative examples 1-4 were tested and the results were as follows.
The prepared Mg-Ta layered composite metal sheet is subjected to surface quality and basal plane yield strength test and field emission electron microscopy (SEM) observation (shown in figure 3), and the Mg-Ta layered composite metal sheet prepared in the example 1 is found to have good surface quality, no obvious cracks at the edge, 130MPa of Mg-Ta layered composite metal sheet interface yield strength, 14 mu m of Mg-Ta layered composite metal sheet interface diffusion width and good interface bonding.
The prepared Mg-Ta layered composite metal sheet is subjected to surface quality and basal plane yield strength test and field emission electron microscopy (SEM) observation (as shown in figure 4), and the surface quality of the Mg-Ta layered composite metal sheet prepared in the example 2 is good, no obvious cracks are formed on the edge, the interfacial yield strength of the Mg-Ta layered composite metal sheet is 150MPa, the interfacial diffusion width of the Mg/Ta layered composite plate is 13.5 mu m, and the interfacial bonding is good.
The Mg-Ta layered composite metal sheet prepared in comparative example 1 was cracked in the process of cutting a tensile sample, the cracking position was located at the center, indicating that the intermediate part of Mg and Ta failed to form effective bonding, indicating that the surface roughening 2-1 of the pure Ta sheet 2 was a key factor in successful preparation of the Mg-Ta layered composite metal sheet of the present invention.
The Mg-Ta layered composite metal plate prepared in comparative example 2 has good surface quality, obvious hole defects are formed at the welding interface of the plate, the yield strength of the interface of the Mg-Ta layered composite metal plate is 80MPa, and the diffusion width of the interface of the Mg-Ta layered composite metal plate is 5.2 mu m, which shows that the Al-coated film 2-2 can effectively improve the bonding capability of Mg-Ta.
The Mg-Ta layered composite metal sheet prepared in comparative example 3 has no obvious holes and no welding defects, the interfacial yield strength of the Mg-Ta layered composite metal sheet is 22MPa, and the interfacial diffusion width is 1.2 mu m, which shows that the Al-plated film 2-2 is a key factor for successfully preparing the Mg-Ta layered composite metal sheet in the invention.
The Mg-Ta layered composite metal plate prepared in comparative example 4 has good surface quality, the interfacial yield strength is 81MPa, the interfacial diffusion width is 8.1 mu m, and the beta phase of the surface BCC can effectively improve the bonding capability of Mg-Ta.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Variations or modifications in the various forms will also be apparent to those of ordinary skill in the art in light of the above description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (9)
1. The hot isostatic pressing diffusion connection preparation method of the Mg-Ta layered composite metal plate is characterized by comprising the following steps of:
firstly, polishing surfaces of a plurality of biphase Mg-Li alloy plates and a plurality of pure Ta plates, cleaning and vacuum drying;
step two, carrying out surface roughening, acid washing, cleaning and vacuum drying on the cleaned pure Ta plates obtained in the step one;
plating Al films on the surfaces of the pure Ta plates subjected to the vacuum drying in the step two;
step four, cleaning the cleaned two-phase Mg-Li alloy plates obtained in the step one and the cleaned pure Ta plates coated with the Al film obtained in the step three, carrying out vacuum drying, sequentially and alternately stacking, loading into a sheath for fixation, and vacuumizing to obtain a to-be-pressed piece;
and fifthly, carrying out hot isostatic pressing on the to-be-pressed piece, and removing the sheath to obtain the Mg-Ta layered composite metal plate.
2. The method for preparing the hot isostatic pressing diffusion joint of the Mg-Ta layered composite metal sheet according to claim 1, wherein in the first step,
polishing the surfaces of the biphase Mg-Li alloy plate and the pure Ta plate by adopting an angle grinder;
the cleaning is chemical cleaning;
the temperature of vacuum drying is 100-150 ℃.
3. The method for preparing the hot isostatic pressing diffusion joint of the Mg-Ta layered composite metal sheet according to claim 1, wherein in the second step,
processing threads or bosses on the surface Mao Huawei of the pure Ta plate;
the pickling is to adopt Ta pickling solution to carry out pickling for 20-40s;
the cleaning is that deionized water is used for cleaning firstly, and IPA ultrasonic cleaning is then used;
the temperature of vacuum drying is 100-150 ℃.
4. The method for preparing the hot isostatic pressing diffusion connection of the Mg-Ta layered composite metal plate according to claim 3, wherein in the second step, the process adopted for carrying out surface roughening on the pure Ta plate is turning.
5. The method for preparing the Mg-Ta layered composite metal plate by hot isostatic pressing diffusion connection according to claim 1, wherein in the third step, the Al film plating process is magnetron sputtering, the magnetron sputtering temperature is 18-28 ℃, the magnetron sputtering power is 250-350W, the chamber pressure is 3.5-4.0x10 Torr, the substrate rotating speed is 5-8r/min, and the sputtering rate is 30-40nm/min.
6. The method for preparing the Mg-Ta layered composite metal sheet by hot isostatic pressing diffusion connection according to claim 1, wherein before the third step, the pure Al target material adopted by the Al film plating is subjected to magnetron sputtering to remove surface oxides.
7. The method for preparing the hot isostatic pressing diffusion joint of the Mg-Ta layered composite metal sheet according to claim 1, wherein in the fourth step,
the cleaning is chemical cleaning;
the temperature of vacuum drying is 100-150 ℃.
8. The method for preparing the Mg-Ta layered composite metal sheet by hot isostatic pressing diffusion connection according to claim 1, wherein in the fourth step, after being stacked alternately in sequence, the upper surface is a dual-phase Mg-Li alloy sheet, and the lower surface is a pure Ta sheet.
9. The method for preparing the Mg-Ta layered composite metal sheet by hot isostatic pressing diffusion connection according to claim 1, wherein in the fifth step, the hot isostatic pressing process condition is nitrogen protection, the pressure is 100-120MPa, the temperature is (0.6-0.8) multiplied by 650 ℃ of Mg melting point, and the time is more than 3-5 h.
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| CN117773304A (en) * | 2024-02-27 | 2024-03-29 | 太原理工大学 | Device and method for prefabricating corrugated electromagnetic forming composite board |
| CN117773304B (en) * | 2024-02-27 | 2024-05-14 | 太原理工大学 | Device and method for prefabricating corrugated electromagnetic forming composite board |
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