CN112719564B - Method for preparing intermetallic compound block by strong deformation assisted vacuum diffusion welding - Google Patents

Method for preparing intermetallic compound block by strong deformation assisted vacuum diffusion welding Download PDF

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CN112719564B
CN112719564B CN202011629026.4A CN202011629026A CN112719564B CN 112719564 B CN112719564 B CN 112719564B CN 202011629026 A CN202011629026 A CN 202011629026A CN 112719564 B CN112719564 B CN 112719564B
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intermetallic compound
plastic body
diffusion welding
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vacuum diffusion
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CN112719564A (en
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万龙
刘景麟
黄体方
黄永宪
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Anhui Wanyu Mechanical Equipment Technology Co ltd
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Kunshan Hagong Wanzhou Welding Research Institute Co ltd
Harbin Institute of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/12Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
    • B23K20/122Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/14Preventing or minimising gas access, or using protective gases or vacuum during welding

Abstract

The invention relates to the field of intermetallic compound preparation, in particular to a method for preparing an intermetallic compound block by strong deformation assisted vacuum diffusion welding, which comprises the following steps: the method comprises the following steps: stirring and rubbing the base material I to form a plastic body I; step two: stirring and rubbing the base metal II to form a plastic body II; step three: cutting the plastic body I and the plastic body II into thin sheets; step four: the plastic body I thin slice and the plastic body II thin slice are mutually stacked and subjected to vacuum diffusion welding to form an intermetallic compound; the base material I and the base material II can be subjected to plastic treatment in advance by adopting stirring friction processing to form a plastic body I and a plastic body II, and then the preparation of the intermetallic compound block is realized by a thin-layer material through a vacuum diffusion welding method; the friction stir processing is to cause the inside of the material to generate violent plastic deformation through a rotating stirring head so as to refine grains, because the diffusion rate of atoms along the grain boundary is far higher than that in the crystal.

Description

Method for preparing intermetallic compound block by strong deformation assisted vacuum diffusion welding
Technical Field
The invention relates to the field of intermetallic compound preparation, in particular to a method for preparing an intermetallic compound block by strong deformation assisted vacuum diffusion welding.
Background
The covalent bond in the intermetallic compound enables metal atoms to have stronger bonding force, the metal bonding bond has stronger stability, and the intermetallic compound has the characteristics of high melting point, high hardness, high temperature resistance, oxidation resistance, creep resistance and the like, and is popular in the aerospace field. The intermetallic compound is widely applied to the fields of energy and communication as an electromagnetic material; as a superconducting material, the superconducting critical temperature is greatly improved, and a wide space is opened up for the application of the superconducting material. In addition, the hydrogen storage capacity of the intermetallic compound is tens of times better than that of the gas cylinder. With the increasing demand of intermetallic compounds, how to produce intermetallic compounds with high quality and high efficiency has become a problem to be solved.
At present, the preparation of intermetallic compounds usually adopts mechanical alloying, self-propagating high-temperature synthesis, spark plasma sintering, directional solidification technology and hot isostatic pressing method. However, the above-mentioned methods all have some drawbacks such as agglomeration, high solubility defect, large porosity, low production efficiency, and difficulty in preparing intermetallic compounds having large size.
The mechanical alloying method usually produces agglomeration phenomenon during the preparation of intermetallic compounds, and influences the unbalanced structure and the performance.
The self-propagating high-temperature synthesis technology has extremely high temperature gradient in the heating and cooling process of preparing intermetallic compounds, so that the material generates high-concentration defects. In addition, too high a heat of reaction causes the material to have a large porosity.
The spark plasma sintering technique has difficulty in preparing intermetallic compounds having a large size due to the functionality of the device and the pulse current capacity. In addition, the graphite mold has high cost and low strength.
In summary, the prior art has the disadvantage that sufficient atomic interdiffusion between stacked layers cannot be achieved in a short time, and the preparation of intermetallic compound bulk is achieved.
Disclosure of Invention
The invention aims to provide a method for preparing an intermetallic compound block by strong deformation assisted vacuum diffusion welding, which can realize sufficient atomic interdiffusion among laminated materials in a short time and realize the preparation of the intermetallic compound block.
The purpose of the invention is realized by the following technical scheme:
a method for preparing an intermetallic compound block by strong deformation assisted vacuum diffusion welding comprises the following steps:
the method comprises the following steps: stirring and rubbing the base material I to form a plastic body I;
step two: stirring and rubbing the base metal II to form a plastic body II;
step three: cutting the plastic body I and the plastic body II into thin sheets;
step four: and the plastic body I thin sheet and the plastic body II thin sheet are mutually overlapped and subjected to vacuum diffusion welding to form an intermetallic compound.
As further optimization of the technical scheme, the method for preparing the intermetallic compound block by strong deformation assisted vacuum diffusion welding comprises the following steps of:
the method comprises the following steps: the base metal I is clamped on a workbench of a friction stir welding machine;
step two: and (3) performing multi-pass processing on the base material I by adopting a stirring friction processing technology to form a plastic body I.
As further optimization of the technical scheme, the method for preparing the intermetallic compound block by strong deformation assisted vacuum diffusion welding comprises the following steps of:
the method comprises the following steps: the base metal II is clamped on a workbench of the friction stir welding machine;
step two: and performing multi-pass processing on the base material II by adopting a stirring friction processing technology to form a plastic body II.
As further optimization of the technical scheme, the method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding has the advantages that the length and the width of the thin sheet prepared by cutting the plastic body I and the plastic body II are the same.
As further optimization of the technical scheme, the method for preparing the intermetallic compound block by the aid of the strong deformation and the vacuum diffusion welding determines the thicknesses of the cut sheets of the plastic body I and the plastic body II according to the component proportion of the intermetallic compound.
As a further optimization of the technical scheme, the method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding has the advantages that the base material I is provided with a plurality of types, the base materials I are respectively provided with different metal materials, the base material II is provided with a plurality of types, and the base materials II are respectively provided with different metal materials.
As a further optimization of the technical scheme, the method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding has the advantages that the base metal I and the base metal II are both made of metal materials which can be subjected to friction stir processing and can generate intermetallic compounds.
As further optimization of the technical scheme, the invention discloses a method for preparing an intermetallic compound block by strong deformation assisted vacuum diffusion welding, which comprises the following steps:
the method comprises the following steps: placing the laminated sheets on a clamp in a vacuum diffusion welding furnace and clamping, then closing a furnace door and opening an air suction pump to extract air in a furnace chamber of the vacuum diffusion welding furnace so as to form a vacuum environment;
step two: starting a cylinder so as to apply certain pressure on the surface of the laminated structure to ensure that no pores are generated in the preparation of the intermetallic compound;
step three: starting the heating function of the vacuum diffusion welding furnace, rapidly heating the heating furnace to the reaction temperature, and keeping the temperature for 5-300 min;
step four: and after the heat preservation is finished, cooling to room temperature along with the furnace and taking out the block to obtain the required intermetallic compound.
As further optimization of the technical scheme, the method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding searches the reaction temperature of the intermetallic compound to be prepared in the alloy phase diagram and sets the temperature as the heating temperature of the vacuum diffusion welding furnace.
The method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding has the beneficial effects that:
the invention relates to a method for preparing an intermetallic compound block by strong deformation assisted vacuum diffusion welding, which can adopt stirring friction processing to perform plastic treatment on a base material I and a base material II in advance to form a plastic body I and a plastic body II, and then a thin layer material realizes the preparation of the intermetallic compound block by a vacuum diffusion welding method; the stirring and rubbing processing is that the inside of the material is subjected to violent plastic deformation through a rotating stirring head, so that crystal grains are refined, and the diffusion rate of atoms along the grain boundary is far higher than that of atoms in the crystal; therefore, the grain refinement is beneficial to promoting the atomic diffusion of the material, and then the plasticized material is cut into thin layers and then the thin-layer materials are quickly and fully interdiffused through vacuum diffusion welding to prepare the intermetallic compound block, so that the required diffusion welding time and the requirement are lower; therefore, the method has the advantages of no oxidation, no agglomeration, capability of preparing the intermetallic compound with larger size and capability of preparing a plurality of intermetallic compound blocks at one time.
Drawings
The invention is described in further detail below with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a schematic structural view of a base material I of the present invention;
FIG. 2 is a schematic structural view of a base metal II according to the present invention;
FIG. 3 is a schematic diagram of a first process for preparing a plastic body by friction stir processing according to the present invention;
FIG. 4 is a schematic diagram of a second process for preparing a plastic body by friction stir processing of the present invention;
FIG. 5 is a schematic diagram of the preparation of intermetallic compounds in the vacuum diffusion welding furnace of the present invention.
In the figure: a base material I1; a base material II 2; a stirring tool 3; a plastomer I4; a plastomer II 5; pressure 6; a vacuum environment 7.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The first embodiment is as follows:
in the following, referring to fig. 1 to 5, the present embodiment is described, and a method for preparing an intermetallic compound bulk by strong deformation assisted vacuum diffusion welding includes the following steps:
the method comprises the following steps: stirring, rubbing and processing the base material I1 to form a plastic body I4;
step two: stirring and rubbing the base material II 2 to form a plastic body II 5;
step three: cutting the plastic body I4 and the plastic body II 5 into thin sheets; wherein the thickness of the prepared sheet is 0.5-2 mm. And finishing the thin sheet by a grinding machine to ensure the thickness accuracy of the processed sheet-shaped body. Wherein the thickness of the sheet processed by the grinding machine is 1 mu m-1 mm.
Step four: the plastic body I4 thin sheet and the plastic body II 5 thin sheet are mutually stacked and subjected to vacuum diffusion welding to form an intermetallic compound; the intermetallic compound produced may comprise two elements, or even more than two elements.
The second embodiment is as follows:
in the following description of the present embodiment with reference to fig. 1 to 5, the first embodiment is further described, in which the step of forming the plastic body i 4 by friction stir processing of the base material i 1 is:
the method comprises the following steps: the base metal I1 is clamped on a workbench of a friction stir welding machine;
step two: performing multi-pass processing on the base material I1 by adopting a stirring friction processing technology to form a plastic body I4; setting the welding speed to be 5-6000 mm/min, setting the rotating speed to be 50-5000 rpm, and setting the pressing amount of the shaft shoulder to be 0-1 mm; when the thickness of the base material I1 is smaller than 2mm, a needleless stirring head can be selected for processing; when the thickness of the base material I1 is larger, a pin stirring head is adopted for processing. The friction stir processing can refine the grains, thereby increasing vacancies and dislocations and providing channels for the diffusion between atoms. In order to improve the processing efficiency, grooves such as threads and the like can be processed on the stirring pin to promote the material flow property.
The third concrete implementation mode:
the present embodiment will be described with reference to fig. 1 to 5, and the second embodiment will be further described, in which the step of forming the plastic body ii 5 by friction stir processing of the base material ii 2 is:
the method comprises the following steps: the base metal II 2 is clamped on a workbench of the friction stir welding machine;
step two: performing multi-pass processing on the base material II 2 by adopting a stirring friction processing technology to form a plastic body II 5; setting the welding speed to be 5-6000 mm/min, setting the rotating speed to be 50-5000 rpm, and setting the pressing amount of the shaft shoulder to be 0-1 mm; when the thickness of the base material II 2 is less than 2mm, a needleless stirring head can be selected for processing; when the base material II 2 is thick, a pin stirring head is adopted for processing. The friction stir processing can refine the grains, thereby increasing vacancies and dislocations and providing channels for the diffusion between atoms. In order to improve the processing efficiency, grooves such as threads and the like can be processed on the stirring pin to promote the material flow property.
The fourth concrete implementation mode:
the present embodiment will be described with reference to fig. 1 to 5, and the third embodiment will be further described, in which plastomer i 4 and plastomer ii 5 are cut into sheets having the same length and width;
the relationship between the number of atoms and the volume is:
n (atomic number) ═ ρ (material density) × V (sheet volume) × NA(avogalois)/M (molar mass), the calculation of the number of atoms can be converted to a volume calculation, which facilitates the preparation of the flakes.
In particular, since the preparation of intermetallic compounds requires the length and width dimensions of the flakes to be the same, the relationship between the number of atoms of the two metals and the thickness of the flakes is:
Figure BDA0002879718170000061
the fifth concrete implementation mode:
the present embodiment will be described with reference to fig. 1 to 5, and the present embodiment will further describe embodiment four in which the thicknesses of cut sheets of plastomer i 4 and plastomer ii 5 are determined in accordance with the respective component ratios of the intermetallic compound.
The sixth specific implementation mode:
the present embodiment will be described with reference to fig. 1 to 5, and the present embodiment will further describe a fifth embodiment in which a plurality of base materials i 1 are provided, a plurality of base materials i 1 are provided as different metal materials, respectively, a plurality of base materials ii 2 are provided, and a plurality of base materials ii 2 are provided as different metal materials, respectively; the design can be carried out according to the type of the intermetallic compound preparation, different types of intermetallic compounds are prepared on the lower part and the upper part, and the preparation of the gradient functional material is realized by a strong deformation assisted vacuum diffusion welding method; when the intermetallic compound with larger brittleness is prepared, the metal with stronger toughness can be added in the middle, and the composite structure is prepared by a strong deformation auxiliary vacuum diffusion welding method; the stirring friction processing can be carried out on the base material I or the base material II 2 only, so that the one-way atom diffusion capacity is enhanced, the speed difference between the two atoms is small, and the generation of Kendall holes is avoided.
The seventh embodiment:
in the sixth embodiment, the present embodiment will be described with reference to fig. 1 to 5, and both the base material i 1 and the base material ii 2 are metallic materials that can be friction stir processed and that can form an intermetallic compound.
The specific implementation mode is eight:
the present embodiment will be described below with reference to fig. 1 to 5, and a seventh embodiment will be further described in the present embodiment, in which the vacuum diffusion welding step is:
the method comprises the following steps: placing the laminated sheets on a clamp in a vacuum diffusion welding furnace and clamping, then closing a furnace door and opening an air suction pump to extract air in a furnace chamber of the vacuum diffusion welding furnace to form a vacuum environment 7; wherein the vacuum degree in the furnace chamber after air extraction is 5 × 10-4~0.1Pa。
Step two: starting the cylinder, so as to apply certain pressure 6 on the surface of the laminated structure to ensure that no pores are generated in the preparation of the intermetallic compound; the pressure applied by the air cylinder is 5-40 MPa.
Step three: starting the heating function of the vacuum diffusion welding furnace, rapidly heating the heating furnace to the reaction temperature, and keeping the temperature for 5-300 min;
step four: and after the heat preservation is finished, cooling to room temperature along with the furnace and taking out the block to obtain the required intermetallic compound.
The specific implementation method nine:
the present embodiment will be described with reference to fig. 1 to 5, and the present embodiment will further describe embodiment eight by searching the reaction temperature of the intermetallic compound to be produced in the alloy phase diagram and setting the reaction temperature as the heating temperature of the vacuum diffusion welding furnace.
The invention relates to a method for preparing an intermetallic compound block by strong deformation assisted vacuum diffusion welding, which comprises the following working processes:
the steps for preparing the FeAl intermetallic compound are as follows:
the method comprises the following steps: according to the preparation of the FeAl intermetallic compound, two iron plates with the thickness of 8mm and one aluminum material are selected as parent materials. And clamping the plate on a workbench of a friction stir welding machine and performing multi-pass processing on the base metal by adopting a friction stir processing technology. Stopping and detaching the plate when the whole plate is processed;
specifically, the Al welding speed was set to 10mm/min, the rotation speed was set to 400rpm, and the shoulder depression amount was 0.1 mm; the Fe welding speed was 100mm/min, the rotation speed was set at 600rpm, and the shoulder depression amount was 0.2 mm.
Preferably, the diameter of a shaft shoulder of the stirring head is 20mm, the length of the needle is 7.8mm, the diameter of the root of the conical needle is 8mm, and the diameter of the tip of the conical needle is 3.5mm, wherein the stirring head is made of tungsten-rhenium alloy;
step two: and respectively cutting the processed aluminum and iron sheets into sheets with the thicknesses of 0.9mm and 0.8mm by a mechanical processing mode. After the grinding machine processing, the final thickness of the aluminum and iron sheets is 0.7mm and 0.5mm respectively.
Step three: arranging the two slices in a mode of Fe-Al-Fe-Al-Fe-Al-Fe-Al-Fe-Al-Fe-Al-Fe-Al;
step four: and (3) placing the laminated sheets on a clamp in a vacuum diffusion welding furnace and clamping, then closing the furnace door and opening an air suction pump to suck the air in the furnace chamber of the vacuum diffusion welding furnace to enable the furnace chamber to be in a vacuum state. Wherein the vacuum degree in the furnace chamber after air extraction is 2 x 10-3Pa。
Step five: when the vacuum is drawn, the cylinder is started to apply a certain pressure on the surface of the laminated structure so as to ensure that no pores are generated in the preparation of the intermetallic compound. Wherein the pressure applied by the air cylinder is 30 MPa.
Step six: and starting the heating function of the vacuum diffusion welding furnace. The furnace was rapidly warmed to 750 ℃ and held at this temperature for 60 min. And after the heat preservation is finished, cooling to room temperature along with the furnace and taking out the block to obtain the needed intermetallic compound matrix composite structure.
Preparation of TiAl3The procedure for the intermetallic compound was as follows:
the method comprises the following steps: according to the preparation of TiAl3Intermetallic compound ofSelecting two titanium plates with the thickness of 6mm and one aluminum material as base materials. And clamping the plate on a workbench of a friction stir welding machine and performing multi-pass processing on the base metal by adopting a friction stir processing technology. Stopping and detaching the plate when the whole plate is processed;
specifically, the titanium welding speed was set to 50mm/min, the rotation speed was set to 200rpm, and the shoulder depression amount was 0.1 mm; the aluminum welding speed was 300mm/min, the rotational speed was set at 1400rpm, and the shoulder depression amount was 0.1 mm.
Particularly, the diameter of a shaft shoulder of the stirring head is 20mm, the length of a needle is 5.8mm, the diameter of the root of a conical needle is 8mm, and the diameter of the tip of the conical needle is 4mm, wherein the stirring head is made of tungsten-rhenium alloy;
step two: and respectively cutting the processed aluminum and titanium sheets into sheets with the thicknesses of 1.6mm and 1.8mm by a mechanical processing mode. After grinding, the final thickness of the aluminum and titanium sheets is 1.43mm and 0.5mm respectively.
Step three: arranging the two slices in an Al-Ti-Ti-Al-Ti-Ti-Al-Ti mode;
step four: and (3) placing the laminated sheets on a clamp in a vacuum diffusion welding furnace and clamping, then closing the furnace door and opening an air suction pump to suck the air in the furnace chamber of the vacuum diffusion welding furnace to enable the furnace chamber to be in a vacuum state. Wherein the vacuum degree in the furnace chamber after air extraction is 5 × 10-4Pa。
Step five: when the vacuum is drawn, the cylinder is started to apply a certain pressure on the surface of the laminated structure so as to ensure that no pores are generated in the preparation of the intermetallic compound. Wherein the pressure applied by the air cylinder is 20 MPa.
Step six: and starting the heating function of the vacuum diffusion welding furnace. The furnace was rapidly warmed to 900 ℃ and held at this temperature for 5 min. And after the heat preservation is finished, cooling to room temperature along with the furnace and taking out the block to obtain the needed intermetallic compound matrix composite structure.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and that various changes, modifications, additions and substitutions which are within the spirit and scope of the present invention and which may be made by those skilled in the art are also within the scope of the present invention.

Claims (7)

1. A method for preparing an intermetallic compound block by strong deformation assisted vacuum diffusion welding is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: stirring, rubbing and processing the base material I (1) to form a plastic body I (4);
step two: stirring and rubbing the base material II (2) to form a plastic body II (5);
step three: cutting the plastic body I (4) and the plastic body II (5) into thin sheets; determining the thickness of the cut sheet of the plastic body I (4) and the plastic body II (5) according to the component ratio of the intermetallic compound; the base material I (1) is provided with a plurality of types, the base materials I (1) are respectively set to be different metal materials, the base material II (2) is provided with a plurality of types, and the base materials II (2) are respectively set to be different metal materials;
step four: the plastic body I (4) thin sheet and the plastic body II (5) thin sheet are mutually overlapped and subjected to vacuum diffusion welding to form an intermetallic compound.
2. The method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding according to claim 1, wherein the method comprises the following steps: the method for forming the plastic body I (4) by stirring, rubbing and processing the base material I (1) comprises the following steps:
the method comprises the following steps: the base metal I (1) is clamped on a workbench of a friction stir welding machine;
step two: and (3) performing multi-pass processing on the base material I (1) by adopting a stirring friction processing technology to form a plastic body I (4).
3. The method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding according to claim 2, wherein the method comprises the following steps: the method for forming the plastic body II (5) by stirring, rubbing and processing the base material II (2) comprises the following steps:
the method comprises the following steps: the base metal II (2) is clamped on a workbench of the friction stir welding machine;
step two: and (3) performing multi-pass processing on the base material II (2) by adopting a stirring friction processing technology to form a plastic body II (5).
4. The method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding according to claim 1, wherein the method comprises the following steps: plastomer I (4) and plastomer II (5) were cut to produce sheets of the same length and width.
5. The method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding according to claim 1, wherein the method comprises the following steps: the base material I (1) and the base material II (2) are both metal materials which can be subjected to friction stir processing and can generate intermetallic compounds.
6. The method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding according to claim 1, wherein the method comprises the following steps: the vacuum diffusion welding comprises the following steps:
the method comprises the following steps: placing the laminated sheets on a clamp in a vacuum diffusion welding furnace and clamping, then closing a furnace door and opening an air suction pump to extract air in a furnace chamber of the vacuum diffusion welding furnace so as to form a vacuum environment (7);
step two: starting the cylinder, so as to apply a certain pressure (6) on the surface of the laminated structure to ensure that no pores are generated in the preparation of the intermetallic compound;
step three: starting the heating function of the vacuum diffusion welding furnace, rapidly heating the heating furnace to the reaction temperature, and keeping the temperature for 5-300 min;
step four: and after the heat preservation is finished, cooling to room temperature along with the furnace and taking out the block to obtain the required intermetallic compound.
7. The method for preparing the intermetallic compound block by the strong deformation assisted vacuum diffusion welding according to claim 6, wherein the method comprises the following steps: and searching the reaction temperature of the intermetallic compound to be prepared in the alloy phase diagram and setting the temperature as the heating temperature of the vacuum diffusion welding furnace.
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