CN115178914B - For Ti 2 AlNb intermetallic compound diffusion welding high-entropy middle layer and preparation method thereof - Google Patents
For Ti 2 AlNb intermetallic compound diffusion welding high-entropy middle layer and preparation method thereof Download PDFInfo
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/32—Selection of soldering or welding materials proper with the principal constituent melting at more than 1550 degrees C
- B23K35/325—Ti as the principal constituent
-
- 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
-
- 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
- B23K20/14—Preventing or minimising gas access, or using protective gases or vacuum during welding
-
- 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
- B23K20/16—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating with interposition of special material to facilitate connection of the parts, e.g. material for absorbing or producing gas
-
- 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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
Abstract
The invention relates to a method for preparing Ti 2 AlNb intermetallic compound diffusion welding high-entropy intermediate layer and preparation method thereof, in order to solve pure metal intermediate layer Ti 2 The invention provides a preparation method of a high-entropy middle layer capable of inhibiting compound formation, which aims to solve the problem that an AlNb diffusion welding interface brittle compound is enriched and interface brittleness is induced. Firstly preparing an alloy ingot according to the corresponding element proportion by utilizing arc melting, then preparing an intermediate layer with the thickness of 50-80 mu m by adopting a cold rolling, mechanical grinding and polishing method, and finally completing joint welding by utilizing vacuum diffusion welding. Compared with direct diffusion welding, the high-entropy alloy is adopted as the diffusion welding interlayer, and the high-entropy alloy can obviously show an elongated welding line and corresponds to the pure metal interlayer, so that the formation of brittle compounds can be inhibited, solid solution components are kept at interfaces, and the improvement of the comprehensive performance of the interfaces is facilitated. The processing is convenient, and the foil is easy to manufacture.
Description
Technical Field
The invention belongs to the field of metal diffusion welding, and relates to a method for welding Ti 2 A high-entropy intermediate layer for AlNb intermetallic compound diffusion welding and a preparation method thereof, in particular to a method for manufacturing a diffusion welding intermediate layer for Ti2AlNb titanium-based intermetallic compound alloy.
Background
Ti 2 AlNb as a light high-strength high-temperature-resistant intermetallic compound alloy can be obtained byThe service temperature is 600-750 ℃. Compared with GH4169, the density is reduced by more than 35%, the specific strength is improved by 20%, the high-temperature yield strength at 650 ℃ is improved by 15%, and the performance of excellent creep resistance, corrosion resistance and the like is considered, so that the alloy is expected to be used for replacing GH4169 in manufacturing of aerospace high-temperature resistant parts and used for reducing the weight of integral parts, such as blisks, blades and combustion chamber parts in aeroengines. The structure of the parts is complex, and Ti 2 The AlNb alloy is difficult to form at room temperature, the integral forming difficulty of parts is high, the performance is unstable, and the manufacturing cost is high. Thus, integral joining after batch fabrication by a welding process is a common means in the fabrication of such parts.
In the traditional fusion welding mode, ti is in the cooling process after welding due to the severe phase change process accompanied by melting and solidification 2 The brittle strengthening phase O phase in the AlNb matrix is easy to concentrate at the crystal boundary of the molten pool matrix, so that the crystal boundary brittleness is improved, and finally, the brittle fracture along the crystal occurs after welding. The diffusion welding is used as a solid-phase welding method, the whole process does not involve material melting, so that the segregation of the grain boundary of O phase can be effectively avoided, and meanwhile, the method combines excellent joint mechanical property and precise forming precision, thereby becoming aerospace Ti 2 Key links for manufacturing AlNb parts.
At present, ti is 2 Alloy of AlNb is homogeneous, ti 2 Researches on AlNb/TiAl hetero-diffusion welding are reported. With the researchers doing Ti 2 Direct diffusion welding of AlNb, but in the full welding temperature range of 900-1000 ℃, a straight welding line exists at a welding line interface, and finally the joint is subjected to brittle fracture along the welding line. (Y.D.Chu, J.S.Li, L.Zhu, B.Tang, H.C.Kou, characterization of the interfacial-microstructure evolution and void shrinkage of Ti-22Al-25Nb orthorhombic alloy with different surface roughness during diffusion bonding.Intermetallics,90 (2017), 119-127) also has researchers utilized externally applied electric field to assist diffusion welding, which eliminates the weld line, but both the method and the regulation method of directly increasing the welding temperature face the degradation of the parent metal structure, solid solution of O phase, grain growth of matrix B2 phase, and damage of the original forging structure. (Investigation on electrically-assisted diffusion bonding)of Ti2AlNb alloy sheet by microstructural observation,mechanical tests and heat treatment.Materials&Design,2018,157:351-361 (CN 105798449 a) describes a method for achieving diffusion bonding of high niobium TiAl alloys using composite metal foil superposition (Ti/Nb/Ti). The method realizes the effective connection of the TiAl alloy, but because the diffusion of Nb element is slow, even if the welding temperature reaches 1100-1300 ℃, a layer of Nb foil still has no reaction in the central area of the interface, so that the existence of pure Nb can become a weak link of the joint in the subsequent high-temperature service. The patent (CN 114131295A) utilizes a similar method of overlapping metal intermediate layers (Ti/Nb), and realizes Ti at the temperature range of 900-960 ℃ and the welding pressure of 5-25 MPa and the heat preservation for 1h 2 The AlNb/TiAl hetero diffusion joint has good room temperature and high temperature (650 ℃) tensile property, but can be seen from the structure, and the joint is formed by Ti foil and Ti 2 The boundary of the AlNb has a large amount of needle-like structures, the structures are unevenly changed, the possible reasons are that Al element of the matrix is rapidly diffused and reacts with the intermediate layer of the Ti foil to form a compound, and the compound is usually brittle, so that the compound can become a weak point in the subsequent service process. Patent (CN 111421218A) uses a method of preparing a catalyst in advance of Ti 2 Hydrogen is put in AlNb to complete the connection with TC4, but the patent does not give specific joint structure and mechanical property indexes, and the alloy is prepared from Ti 2 TC4 fails due to high temperatures in the service temperature range of AlNb. Patent (CN 109332872A) completes Ti by surface treatment 2 The homogeneous welding of the AlNb, but the organization and mechanical properties of the response are not reported in the patent.
In summary, in order to solve the problem that the interlayer material is easy to react with the matrix Al to form a brittle compound, it is necessary to design a proper alloy interlayer material, so as to eliminate the bonding wire, effectively control the interface reaction, reduce the tendency of compound generation, and thereby comprehensively improve the mechanical properties of the joint. The Ti refractory high-entropy alloy is a new material which has been developed recently, and its own element is designed as a plurality of principal elements, so that it has a hysteresis diffusion effect on the tissue and a cocktail effect on the performance. The most of the materials are IVB, VB, VIBThe group element is composed of bcc structure which is stable at high temperature, has good solid solubility for Al element and excellent high temperature performance, and can meet the requirement of Ti 2 Service requirements of the AlNb alloy.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing Ti 2 AlNb intermetallic compound diffusion welding high-entropy intermediate layer and preparation method thereof, and existing Ti 2 In the AlNb diffusion welding, the problem that the simple substance metal intermediate layer/simple substance metal superposition intermediate layer reacts with the base metal to form brittle compounds.
Technical proposal
For Ti 2 The AlNb intermetallic compound diffusion welding high-entropy intermediate layer is characterized in that the atomic ratio of elements is Nb 45 Ta 25 Ti 15 Hf 15 Elemental purity requirements are greater than 99.9wt.%.
The pure metal element particles Nb, ta, hf, ti are stored in vacuum.
For Ti 2 The preparation method of the AlNb intermetallic compound diffusion welding high-entropy middle layer is characterized by comprising the following steps of:
step 1, alloy component proportion: according to atomic ratio of element Nb 45 Ta 25 Ti 15 Hf 15 Weighing pure metal element particles Nb, ta, hf, ti, cleaning the surface by dilute acid solution, and placing the pure metal element particles in alcohol solution for ultrasonic cleaning;
step 2, arc melting to prepare alloy ingots: placing the metal particles Nb, ta, hf, ti into a copper crucible according to the melting point of the metal particles, wherein the low melting point is placed at the bottom and the high melting point is placed at the top;
adopting an arc melting method, carrying out forward and reverse melting for more than 5 times, and carrying out electromagnetic stirring to obtain a molten ingot;
step 3, cold rolling and preparing a high-entropy middle layer: dividing the molten ingot into cuboid, and polishing the surface to be smooth until the linear cutting trace disappears; coating cold rolling lubricating oil on two sides of a roller, and pressing the roller in a single batch by 0.5-0.25mm; cold rolling the alloy ingot to a thickness of 0.1-0.2mm in batches; sectionally cutting the cold-rolled sheet, polishing the upper and lower surfaces until the overall thickness is 50-80 mu m, mechanically polishing the two surfaces by using polishing solution, wherein the surface roughness is less than Ra0.1;
corroding the surface by using Kaile reagent, and placing in alcohol solution for ultrasonic cleaning for 5-20min, and drying to obtain the high-entropy middle layer.
The weight of single smelting is normally 50-150g, the excessive weight should be smelted in batches, and then a plurality of alloy ingots are fused to ensure the full alloying of metal particles.
The cuboid of the step 3 is 20mm multiplied by 5mm.
And the polishing in the step 3 is sequentially performed by using 240# sand paper, 400# sand paper, 800# sand paper, 1000# sand paper, 1500# sand paper and 2000# sand paper.
The polishing solution in the step 3 adopts SiO2, H2O2=9:1.
If the high-entropy middle layer in the step 3 needs to be stored, after polishing, placing the surface sealing film in a drying dish for storage, and repeating the corrosion and cleaning steps for the subsequent use, wherein the holding time is not longer than 12 hours at most.
The high-entropy interlayer is used for Ti 2 A method for performing diffusion welding on AlNb intermetallic compounds is characterized by comprising the following steps of: placing a high entropy interlayer in Ti 2 Welding in a vacuum diffusion welding furnace in the middle of the AlNb base metal; welding parameters: heating and pressurizing: a first stage of heating the vacuum diffusion welding furnace from room temperature to 300 ℃ at a heating rate of 10 ℃/min; preserving heat at 300 ℃ for 10min; the second stage, heating to 500 ℃ at 10 ℃/min, and preserving heat for 10min; the third stage, heating to 890 ℃ at 10 ℃/min, and preserving heat for 10min; the fourth stage, heating to 900-970 ℃ at 10 ℃/min, and ending the heating; fifth, preserving heat for 1h at 900-970 ℃, and applying pressure of 20-30 MPa; after the heat preservation and pressure maintaining are finished, unloading the pressure in the furnace to 5MPa at a speed of 5-10 MPa/min, and then cooling the sample along with the furnace; after the sample is cooled to room temperature, the pressure is reset to zero, and the welding is completed; throughout the whole step, the vacuum degree in the furnace chamber of the vacuum hot-pressing furnace is always not higher than 5 multiplied by 10 -3 Pa。
Before welding, sequentially polishing the surface to be welded of the base material by using 400# to 2000# abrasive paper, wherein the surface parallelism is not lower than 0.1; and then mechanically polishing with a polishing solution < Ra0.1. And corroding by using Kaile reagent until the surface is slightly whitened, and ultrasonically cleaning for 10min.
Advantageous effects
The invention provides a method for preparing Ti 2 AlNb intermetallic compound diffusion welding high-entropy intermediate layer and preparation method thereof, in order to solve pure metal intermediate layer Ti 2 The invention provides a preparation method of a high-entropy middle layer capable of inhibiting compound formation, which aims to solve the problem that an AlNb diffusion welding interface brittle compound is enriched and interface brittleness is induced. Firstly preparing an alloy ingot according to the corresponding element proportion by utilizing arc melting, then preparing an intermediate layer with the thickness of 50-80 mu m by adopting a cold rolling, mechanical grinding and polishing method, and finally completing joint welding by utilizing vacuum diffusion welding. The preparation method and welding process of the intermediate layer of the invention are as follows: intermediate layer alloy atomic ratio Nb 45 Ta 25 Ti 15 Hf 15 The cold rolling deformation is more than 98%, the grinding and polishing are carried out until the thickness is 50-80 mu m, and the roughness of the two surfaces of the middle layer is less than Ra0.1; the welding temperature rising speed is 10 ℃/min, the welding temperature is 950 ℃, the pressure is 20-30MPa, and the heat preservation and pressure maintaining are carried out for 60min.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with direct diffusion welding, the high-entropy alloy is adopted as the diffusion welding intermediate layer, the high-entropy alloy can obviously show an elongated welding line, and is corresponding to the pure metal intermediate layer, the diffusion of Al element can be reduced by utilizing the hysteresis diffusion effect of the high-entropy alloy, and simultaneously, the ternary phase diagram composed of Nb, ta, hf, ti and Al has great solid solubility for Al, so that the formation of brittle compounds can be inhibited, solid solution components can be kept at interfaces, and the improvement of the comprehensive performance of the interfaces is facilitated.
2. The high-entropy alloy of the invention is composed of a plurality of refractory elements, has high melting point and higher recrystallization temperature, and is prepared from Ti 2 In the service temperature range of AlNb, the structure is stable, no obvious phase change and grain growth exist, the high-temperature material performance is ensured, the high-temperature material has extremely high room temperature deformability, the processing is convenient, and the foil is easy to manufacture.
3. In terms of welding performance, the method provided by the invention adopts Nb 45 Ta 25 Ti 15 Hf 15 High entropy alloyThe foil is used as the middle layer, the components of the middle layer are reasonably optimized, the welding parameters are regulated and controlled, and the Ti is inhibited 2 And separating out interfacial compounds in the AlNb diffusion connection process. On the basis of not reducing the strength, the plasticity is improved by 30 percent compared with the parent metal of a furnace, the tensile sample obviously breaks and the parent metal, the strength of the tensile sample is equal to that of the parent metal, the plasticity reaches the parent metal level due to the level of the parent metal, and the high-temperature tensile strength at 650 ℃ reaches the level of the parent metal, and the weld breaks and the parent metal.
Drawings
FIG. 1 is Ti 2 AlNb diffusion welding interface structure and mechanical property
Detailed Description
The invention will now be further described with reference to examples, figures:
the technical scheme of the invention comprises the following steps:
step one: alloy composition ratio. Pure metal element particles Nb, ta, hf, ti with an element atomic ratio of Nb are weighed by a precision electronic balance 45 Ta 25 Ti 15 Hf 15 The purity of the elements is required to be more than 99.9 wt%, and meanwhile, the alloy particles are stored in vacuum as much as possible, the surfaces of the alloy particles are cleaned by a small amount of dilute acid solution before use, and the alloy particles are placed in alcohol solution for ultrasonic cleaning, so that the cleanliness of the particles is ensured, the impurities are reduced, and the proportioning weight is determined according to the follow-up arc smelting equipment.
Step two: arc melting to prepare alloy ingots. And smelting the metal particles in sequence by using an arc smelting method, wherein the metal particles are sequentially placed in a copper crucible according to the melting point of the element, the low melting point is placed at the bottom, and the high melting point is placed at the top. The positive and negative smelting is carried out for at least 5 times, electromagnetic stirring is carried out to ensure that the particles are melted thoroughly and uniformly, the weight of single smelting is not excessive, the conventional weight is 50-150g, the excessive weight is required to be smelted in batches, and then a plurality of alloy ingots are fused to ensure that the metal particles are fully alloyed.
Step three: and (5) cold rolling the high-entropy middle layer. The ingot is divided into cuboid with 20mm multiplied by 5mm by using a cutting tool (such as a wire cutting machine, a metallographic cutting machine and the like), and the surface is polished and flattened until the wire cutting trace disappears. And (3) coating cold rolling lubricating oil on two sides of the roller, and pressing the roller by 0.2mm in a single batch. The alloy ingot was cold rolled to a thickness of 0.1mm in batches. The cold-rolled sheet is cut in sections, the upper surface and the lower surface of the cold-rolled sheet are polished by 240#, 400#, 800#, 1000#, 1500#, 2000# abrasive paper in sequence until the overall thickness is 50-80 mu m, and the two surfaces of the cold-rolled sheet are mechanically polished by polishing solution (SiO 2: H2O2=9:1), wherein the surface roughness requirement is less than Ra0.1. And then corroding the surface by using Kaile reagent, and placing the surface in an alcohol solution for ultrasonic cleaning for 10min, and drying for later use. If the surface sealing film needs to be stored, the surface sealing film is placed in a drying dish for storage after polishing, and the corrosion and cleaning steps are repeated for subsequent use, wherein the retention time is not longer than 12 hours at most.
Step four: ti (Ti) 2 And (3) carrying out AlNb vacuum diffusion welding. Placing the high-entropy interlayer prepared in the third step in Ti 2 And welding the AlNb base material in the middle in a vacuum diffusion welding furnace. The specific process is as follows:
(1) And (3) sequentially polishing the surface to be welded of the base material by using 400# to 2000# abrasive paper, wherein the surface parallelism is not lower than 0.1. And then mechanically polishing (< Ra0.1) by using the polishing solution in the step three. And corroding by using Kaile reagent until the surface is slightly whitened, and ultrasonically cleaning for 10min.
(2) Heating and pressurizing: a first stage of heating the vacuum diffusion welding furnace from room temperature to 300 ℃ at a heating rate of 10 ℃/min; the temperature is kept at 300 ℃ for 10min.
And in the second stage, heating to 500 ℃ at 10 ℃/min, and preserving heat for 10min.
And in the third stage, heating to 900 ℃ at 10 ℃/min, and preserving heat for 10min.
And in the fourth stage, the temperature is increased to 950 ℃ at 10 ℃/min, and the temperature is increased to the end.
And fifthly, preserving heat for 1h at 950 ℃. Applying 20-30MPa pressure.
After the heat preservation and pressure maintaining are finished, unloading the pressure in the furnace to 5MPa at a speed of 10MPa/min, and then cooling the sample along with the furnace; and (5) after the sample is cooled to room temperature, the pressure is reset to zero, and the welding is completed. In the whole step five, the vacuum degree in the furnace chamber of the vacuum hot pressing furnace is always not higher than 5 multiplied by 10 -3 Pa。
To solve the problem of pure metal interlayer Ti 2 The invention provides a preparation method of a high-entropy middle layer capable of inhibiting compound formation, which aims to solve the problem that an AlNb diffusion welding interface brittle compound is enriched and interface brittleness is induced. Firstly, electricity is utilizedArc smelting to prepare alloy ingot according to corresponding element proportion, cold rolling, mechanical grinding and polishing to prepare intermediate layer of 50-80 μm thickness, and final vacuum diffusion welding to finish joint welding.
Through the scheme, the preparation method and the welding process of the finally determined intermediate layer are as follows: intermediate layer alloy atomic ratio Nb 45 Ta 25 Ti 15 Hf 15 The cold rolling deformation is more than 98%, the grinding and polishing are carried out until the thickness is 50-80 mu m, and the roughness of the two surfaces of the middle layer is less than Ra0.1; the welding temperature rising speed is 10 ℃/min, the welding temperature is 950 ℃, the pressure is 20-30MPa, and the heat preservation and pressure maintaining are carried out for 60min.
Example 1
The embodiment adopts Nb 45 Ta 25 Ti 15 Hf 15 High entropy alloy foil as an intermediate layer for Ti 2 The AlNb alloy is subjected to diffusion welding connection, and the specific steps are as follows:
smelting an interlayer metal: pure metal element particles Nb, ta, hf, ti with an element atomic ratio of Nb are weighed by a precision electronic balance 45 Ta 25 Ti 15 Hf 15 The purity of the elements is required to be more than 99.9 wt%, the elements are sequentially placed in a copper crucible according to the melting point of the elements, the low melting point is placed at the bottom, and the high melting point is placed at the top. And smelting for at least 5 times, and electromagnetically stirring to ensure that the particles are molten and uniform.
Step two, cold rolling and preparing a high-entropy middle layer: the ingot is divided into cuboid with 20mm multiplied by 5mm by using a cutting tool (such as a wire cutting machine, a metallographic cutting machine and the like), and the surface is polished and flattened until the wire cutting trace disappears. And (3) coating cold rolling lubricating oil on two sides of the roller, and pressing the roller by 0.2mm in a single batch. The alloy ingot was cold rolled to a thickness of 0.1mm in batches. The cold-rolled sheet is cut in sections, the upper surface and the lower surface of the cold-rolled sheet are polished by 240#, 400#, 800#, 1000#, 1500#, 2000# abrasive paper in sequence until the overall thickness is 50-80 mu m, and the two surfaces of the cold-rolled sheet are mechanically polished by polishing solution (SiO 2: H2O2=9:1), wherein the surface roughness requirement is less than Ra0.1. And then corroding the surface by using Kaile reagent, and placing the surface in an alcohol solution for ultrasonic cleaning for 10min, and drying for later use.
Step three, ti 2 And (3) AlNb vacuum diffusion welding: will beThe high-entropy middle layer prepared in the third step is placed in Ti 2 And welding the AlNb base material in the middle in a vacuum diffusion welding furnace. The specific process is as follows:
(1) And (3) sequentially polishing the surface to be welded of the base material by using 400# to 2000# abrasive paper, wherein the surface parallelism is not lower than 0.1. And then mechanically polishing (< Ra0.1) by using the polishing solution in the step three. And corroding by using Kaile reagent until the surface is slightly whitened, and ultrasonically cleaning for 10min.
(2) Heating and pressurizing: a first stage of heating the vacuum diffusion welding furnace from room temperature to 300 ℃ at a heating rate of 10 ℃/min; the temperature is kept at 300 ℃ for 10min.
And in the second stage, heating to 500 ℃ at 10 ℃/min, and preserving heat for 10min.
And in the third stage, heating to 900 ℃ at 10 ℃/min, and preserving heat for 10min.
And in the fourth stage, the temperature is increased to 950 ℃ at 10 ℃/min, and the temperature is increased to the end.
And fifthly, preserving heat for 1h at 950 ℃. Applying 20-30MPa pressure.
After the heat preservation and pressure maintaining are finished, unloading the pressure in the furnace to 5MPa at a speed of 10MPa/min, and then cooling the sample along with the furnace; and (5) after the sample is cooled to room temperature, the pressure is reset to zero, and the welding is completed. In the whole step five, the vacuum degree in the furnace chamber of the vacuum hot pressing furnace is always not higher than 5 multiplied by 10 -3 Pa。
Example two
In the first step, a high-entropy alloy ingot is obtained by adopting an induction smelting method, and the component proportion Nb 40 Ta 25 Ti 20 Hf 15 The remainder was the same as case one.
Example III
In the first step, a method of magnetron sputtering is adopted, and a high-entropy alloy (Nb 45 Ta 25 Ti 15 Hf 15 ) Depositing on the surface of the welded base material, ultrasonically cleaning the surface with alcohol to obtain an intermediate layer with the thickness of 10-15 mu m, and the rest is the same as the first case.
Example IV
The first step adopts a vacuum plasma beam smelting method, and the component Al 5 (Nb 45 Ta 25 Ti 15 Hf 15 ) 95, the welding temperature is increased to970 ℃, and the pressure is 30MPa. The remainder was the same as case one.
Example five
The welding temperature in the fourth step is 900 ℃, the welding time is prolonged to 120min, and the rest is the same as the first case.
Example six
And in the fourth step, a power-on heating mode is adopted, the welding temperature is 970 ℃, the pressure is 30MPa, the welding time is 5min, and the rest is the same as the first case.
Claims (10)
1. For Ti 2 The AlNb intermetallic compound diffusion welding high-entropy intermediate layer is characterized in that the atomic ratio of elements is Nb 45 Ta 25 Ti 15 Hf 15 Elemental purity requirements greater than 99.9wt.%;
said composition is used for Ti 2 The AlNb intermetallic compound diffusion welding high-entropy middle layer is prepared according to the following steps:
step 1, alloy component proportion: according to atomic ratio of element Nb 45 Ta 25 Ti 15 Hf 15 Weighing pure metal element particles Nb, ta, hf, ti, cleaning the surface by dilute acid solution, and placing the pure metal element particles in alcohol solution for ultrasonic cleaning;
step 2, arc melting to prepare alloy ingots: placing the metal particles Nb, ta, hf, ti into a copper crucible according to the melting point of the metal particles, wherein the low melting point is placed at the bottom and the high melting point is placed at the top;
adopting an arc melting method, carrying out forward and reverse melting for more than 5 times, and carrying out electromagnetic stirring to obtain a molten ingot;
step 3, cold rolling and preparing a high-entropy middle layer: dividing the molten ingot into cuboid, and polishing the surface to be smooth until the linear cutting trace disappears; coating cold rolling lubricating oil on two sides of a roller, and pressing the roller in a single batch by 0.5-0.25mm; cold rolling the alloy ingot to a thickness of 0.1-0.2mm in batches; sectionally cutting the cold-rolled sheet, polishing the upper and lower surfaces until the overall thickness is 50-80 mu m, mechanically polishing the two surfaces by using polishing solution, wherein the surface roughness is less than Ra0.1;
corroding the surface by using Kaile reagent, and placing in alcohol solution for ultrasonic cleaning for 5-20min, and drying to obtain the high-entropy middle layer.
2. The method according to claim 1 for Ti 2 The AlNb intermetallic compound diffusion welding high-entropy intermediate layer is characterized in that: the pure metal element particles Nb, ta, hf, ti are stored in vacuum.
3. A method according to claim 1 or 2 for Ti 2 The preparation method of the AlNb intermetallic compound diffusion welding high-entropy middle layer is characterized by comprising the following steps of:
step 1, alloy component proportion: according to atomic ratio of element Nb 45 Ta 25 Ti 15 Hf 15 Weighing pure metal element particles Nb, ta, hf, ti, cleaning the surface by dilute acid solution, and placing the pure metal element particles in alcohol solution for ultrasonic cleaning;
step 2, arc melting to prepare alloy ingots: placing the metal particles Nb, ta, hf, ti into a copper crucible according to the melting point of the metal particles, wherein the low melting point is placed at the bottom and the high melting point is placed at the top;
adopting an arc melting method, carrying out forward and reverse melting for more than 5 times, and carrying out electromagnetic stirring to obtain a molten ingot;
step 3, cold rolling and preparing a high-entropy middle layer: dividing the molten ingot into cuboid, and polishing the surface to be smooth until the linear cutting trace disappears; coating cold rolling lubricating oil on two sides of a roller, and pressing the roller in a single batch by 0.5-0.25mm; cold rolling the alloy ingot to a thickness of 0.1-0.2mm in batches; sectionally cutting the cold-rolled sheet, polishing the upper and lower surfaces until the overall thickness is 50-80 mu m, mechanically polishing the two surfaces by using polishing solution, wherein the surface roughness is less than Ra0.1;
corroding the surface by using Kaile reagent, and placing in alcohol solution for ultrasonic cleaning for 5-20min, and drying to obtain the high-entropy middle layer.
4. A method according to claim 3, characterized in that: the weight of single smelting is normally 50-150g, the excessive weight should be smelted in batches, and then a plurality of alloy ingots are fused to ensure the full alloying of metal particles.
5. A method according to claim 3, characterized in that: the cuboid of the step 3 is 20mm multiplied by 5mm.
6. A method according to claim 3, characterized in that: and the polishing in the step 3 is sequentially performed by using 240# sand paper, 400# sand paper, 800# sand paper, 1000# sand paper, 1500# sand paper and 2000# sand paper.
7. A method according to claim 3, characterized in that: the polishing solution in the step 3 adopts SiO 2 :H 2 O 2 ＝9:1。
8. A method according to claim 3, characterized in that: if the high-entropy middle layer in the step 3 needs to be stored, after polishing, placing the surface sealing film in a drying dish for storage, and repeating the corrosion and cleaning steps for the subsequent use, wherein the holding time is not longer than 12 hours at most.
9. Use of the high entropy interlayer of claim 1 for Ti 2 A method for performing diffusion welding on AlNb intermetallic compounds is characterized by comprising the following steps of: placing a high entropy interlayer in Ti 2 Welding in a vacuum diffusion welding furnace in the middle of the AlNb base metal; welding parameters: heating and pressurizing: a first stage of heating the vacuum diffusion welding furnace from room temperature to 300 ℃ at a heating rate of 10 ℃/min; preserving heat at 300 ℃ for 10min; the second stage, heating to 500 ℃ at 10 ℃/min, and preserving heat for 10min; the third stage, heating to 890 ℃ at 10 ℃/min, and preserving heat for 10min; the fourth stage, heating to 900-970 ℃ at 10 ℃/min, and ending the heating; fifth, preserving heat for 1h at 900-970 ℃, and applying pressure of 20-30 MPa; after the heat preservation and pressure maintaining are finished, unloading the pressure in the furnace to 5MPa at a speed of 5-10 MPa/min, and then cooling the sample along with the furnace; after the sample is cooled to room temperature, the pressure is reset to zero, and the welding is completed; throughout the whole step, the vacuum degree in the furnace chamber of the vacuum hot-pressing furnace is always not higher than 5 multiplied by 10 -3 Pa。
10. The method according to claim 9, wherein: before welding, sequentially polishing the surface to be welded of the base material by using 400# to 2000# abrasive paper, wherein the surface parallelism is not lower than 0.1; mechanically polishing with polishing solution < Ra0.1;
and corroding by using Kaile reagent until the surface is slightly whitened, and ultrasonically cleaning for 10min.
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