CN109396631B - Hot isostatic pressing diffusion bonding method for tungsten/transition layer/stainless steel - Google Patents
Hot isostatic pressing diffusion bonding method for tungsten/transition layer/stainless steel Download PDFInfo
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- CN109396631B CN109396631B CN201811350980.2A CN201811350980A CN109396631B CN 109396631 B CN109396631 B CN 109396631B CN 201811350980 A CN201811350980 A CN 201811350980A CN 109396631 B CN109396631 B CN 109396631B
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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
- B23K20/001—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by extrusion or drawing
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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
- B23K20/021—Isostatic pressure welding
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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
- B23K20/22—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded
Abstract
The invention discloses a hot isostatic pressing diffusion connection method of tungsten/transition layer/stainless steel, which solves the problem that a tungsten and steel connecting piece used for a plasma divertor module facing a first wall of a fusion reactor in the prior art is easy to form larger thermal stress and micro defects on an interface. The invention relates to a hot isostatic pressing diffusion connection method of tungsten/transition layer/stainless steel, which takes pure tungsten, the transition layer and the stainless steel as raw materials, and the hot isostatic pressing diffusion connection piece can be obtained after the cladding treatment, the hot isostatic pressing treatment, the stress relief annealing and the de-cladding. The method is simple to operate, can realize defect-free metallurgical bonding, and has excellent and stable joint performance.
Description
Technical Field
The invention belongs to the technical field of metal material interface connection preparation, and particularly relates to a hot isostatic pressing diffusion connection method of tungsten/transition layer/stainless steel.
Background
The nuclear fusion energy is called as artificial solar energy due to the characteristics of high efficiency, cleanness, safety, rich raw material resources and the like, and is one of the currently recognized important ways of finally solving the energy problem and the environmental problem of the human society and promoting the sustainable development of the human society. The development of nuclear fusion energy has important strategic and economic significance for the sustainable development of China.
At present, one of the key problems restricting the research of nuclear fusion reactors is the preparation of divertors. The divertor is used as a core component of the nuclear fusion reactor and is positioned in a transition zone between high-temperature plasma and common solid materials, and the main components comprise a plasma-facing material, a heat sink material and a structural material. Because the components of the divertor are in different working environments, the performance requirements of the materials are different accordingly. Tungsten is considered to be the most promising plasma-oriented material because of its excellent properties such as high thermal conductivity, high temperature resistance, resistance to sputtering, and low deuterium-tritium adsorption. Low activation steel is considered to be an ideal material for application to structural materials and heat sink materials due to its good resistance to radiation expansion, oxidation, high temperature mechanical properties, and economy. Therefore, successfully joining tungsten and steel together and providing them with certain performance properties is critical to the preparation of divertors.
The key problem of tungsten steel diffusion bonding is that tungsten has a large difference in melting point (Tw 3400 ℃, TS ═ 1500 ℃) and a large difference in thermal expansion coefficient (the thermal expansion coefficient of tungsten is 4.4 × 10-6 · K-1, and the thermal expansion coefficient of steel is 12 × 10-6 · K-1), which results in large residual stress at the joint interface and makes it difficult to bond them by conventional fusion welding. At present, the connection method of tungsten and steel mainly comprises high-temperature brazing connection and diffusion welding connection. High temperature brazing and diffusion welding connections tend to develop large thermal stresses and microscopic defects at the interface. To achieve better heat transfer properties, tungsten steel joints must achieve a defect free metallurgical bond interface.
CN106181015A discloses a manufacturing process method of a first wall part with a tungsten-attached U-shaped flow channel suitable for a fusion reactor cladding, and tungsten and U-shaped flow channel-containing steel are compounded together by a hot isostatic pressing diffusion welding technology to realize functionalization. The patent only proposes one conceptual idea for the combination of tungsten and steel. The sheath welding in the atmospheric environment can cause the surface to be welded to be oxidized due to too high temperature; in addition, the coating is a porous non-compact material, and the adsorbed air is still difficult to be completely desorbed during thermal degassing and is still oxidized or remains on the interface to reduce the performance. In addition, the soldering temperature of this document is significantly too low so that the interdiffusion of the interface elements is insufficient and the bonding strength is low.
Therefore, it is an urgent need to solve the problems of the art to provide a tungsten steel connection method which is simple to operate, can realize defect-free metallurgical bonding, and has excellent and stable joint performance.
Disclosure of Invention
The technical problem solved by the invention is as follows: the hot isostatic pressing diffusion connection method for the tungsten/transition layer/stainless steel solves the problem that a tungsten and steel connecting piece used for facing a plasma divertor module of a first wall of a fusion reactor in the prior art is easy to form large thermal stress and micro defects on an interface.
The technical scheme adopted by the invention is as follows:
the hot isostatic pressing diffusion connection method of tungsten/transition layer/stainless steel, provided by the invention, comprises the steps of using pure tungsten, the transition layer and stainless steel as raw materials, performing canning treatment, then performing hot isostatic pressing treatment, stress relief annealing and canning removal, and thus obtaining the hot isostatic pressing diffusion connection piece.
Further, the method comprises the following steps:
step 1, assembling: sequentially filling pure tungsten, the transition layer and the stainless steel into a sheath;
step 2, welding: welding the sheath assembled in the step 1 with a sheath cover with an exhaust tube to manufacture a sheath assembly;
and step 3, leak detection: detecting leakage of the sheath assembly prepared in the step 2;
step 4, thermal degassing: placing the sheath assembly qualified in the leak detection in the step 3 into a muffle furnace for thermal degassing;
and step 5, sealing: heating and clamping the exhaust pipe on the sheath assembly after the step 4;
step 6, hot isostatic pressing connection: placing the sheath assembly processed in the step 5 in a hot isostatic pressing machine, and performing diffusion connection on tungsten steel sealed in the sheath;
step 7, stress relief annealing: performing stress relief annealing in a hot isostatic pressing machine;
step 8, removing the sheath: and (4) turning the sheath assembly annealed in the step (7) to remove sheath materials, thus obtaining the hot isostatic pressing diffusion connecting piece.
Further, before assembling, the method also comprises the following surface treatment steps: grinding and polishing the surfaces to be connected of the pure tungsten, the transition layer and the stainless steel to a mirror surface by using abrasive paper; and after polishing, ultrasonic cleaning is carried out for 10-30 minutes by alcohol and acetone in sequence.
Further, the pure tungsten is more than 99.5% of tungsten by mass percent; the transition layer is selected from one of single transition layers of copper foil, nickel foil and titanium foil, or is a composite transition layer of copper foil and nickel foil, the mass percentage of the transition layer is more than 99.8%, and the thickness of the transition layer is 0.1 mm-0.5 mm.
Further, the material of the sheath, the sheath cover and the exhaust tube is selected from any one of 08F iron sheet, 1Cr18Ni9Ti steel and 316L stainless steel.
Further, the welding in the step 2 is argon arc welding in a low-oxygen low-humidity argon protection glove box; or electron beam welding in a high vacuum chamber.
Further, step 2 is protecting H in the glove box during argon arc welding2Both the O content and the O content are lower than 10 ppm; step 2 is that when the electron beam welding is carried out, the vacuum degree in the high vacuum chamber is more than 4 multiplied by 10-3Pa。
Further, the hot isostatic pressing diffusion bonding in the step 6 specifically comprises: adopting a mode of pressurizing first and then heating, and starting to heat after the initial pressure is pressurized to 50-60 MPa; the heat preservation time is 30min to 120min, and the hot isostatic pressure is 130MPa to 160 MPa.
Further, when the transition layer is a copper foil, the hot isostatic pressing temperature in the step 6 is 1000-1050 ℃;
when the transition layer is a nickel foil, the hot isostatic pressing temperature in the step 6 is 1300-1350 ℃;
when the transition layer is a titanium foil, the hot isostatic pressing temperature in the step 6 is 1250-1350 ℃;
when the transition layer is a copper foil and nickel foil composite layer, the hot isostatic pressing temperature in the step 6 is 950-1050 ℃.
Further, in the step 7, when the temperature of the workpiece in the hot isostatic pressing machine is reduced to 500-600 ℃, the return gas is uniformly pressurized to normal pressure, and then the temperature is maintained for 30min for stress relief annealing.
The pure tungsten in the step 1 is a pure tungsten block, and the stainless steel is a stainless steel block.
Compared with the prior art, the invention has the following beneficial effects:
the invention has scientific design and simple and convenient operation, promotes the atomic diffusion of the connecting interface material through the combined action of high temperature and high pressure, adopts a proper transition layer and process to avoid the generation of brittle phase, effectively relieves the residual stress of the interface by utilizing stress relief annealing, effectively solves the technical problems of interface pollution, residual stress, brittle phase, micro defect and the like, and obtains the joint with uniform diffusion of elements, realizes the metallurgical bonding without defects, excellent and stable performance and positive engineering use value.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The leak detection in the invention is realized by connecting a helium mass spectrometer leak detector with an air exhaust duct on a sheath end cover.
Example 1
The embodiment provides a preparation method of the invention, which specifically comprises the following steps:
the method comprises the steps of sequentially grinding phi 25 multiplied by 20mm pure tungsten with the purity of 99.5 wt%, phi 25 multiplied by 0.25mm copper foil with the purity of 99.9 wt% and phi 25 multiplied by 20 316L steel with the purity of phi 25 multiplied by 20 through 200 meshes, 400 meshes, 600 meshes, 1000 meshes and 2000 meshes of sand paper, polishing the polished surface of the polished surface through diamond particles with the particle size of 2-5 mu m in water, and sequentially and respectively ultrasonically cleaning the polished surface through alcohol and acetone for 30 minutes.
Sequentially putting the cleaned pure tungsten, copper foil and 316L stainless steel into a sheath of 1Cr18Ni9Ti, and covering the sheath and the sheath with an exhaust tube on a H2Both the O content and the O content are less than 10ppmArgon arc welding is adopted in the low-oxygen low-humidity argon atmosphere glove box to weld the sheathing component, wherein the exhaust tube and the sheathing cover are made of 1Cr18Ni9Ti material. After welding, the sheath is subjected to leak detection with the leak rate less than or equal to 3 multiplied by 10-9Pa·m3/s。
Placing the sheath assembly qualified for leak detection in a muffle furnace, connecting an exhaust pipe on a sheath cover with a high vacuum exhaust system, and performing integral heating and degassing on the sheath assembly at 700 ℃ by using the muffle furnace for 1 hour, wherein the vacuum degree in the process is better than 3 x 10-3Pa. And heating and clamping the exhaust pipe covered on the sheath for three times from the sheath assembly from near to far.
And (3) placing the sheathed assembly subjected to heating and clamping in a hot isostatic pressing machine for diffusion connection, wherein the hot isostatic pressing temperature is 1050 ℃, the pressure is 152MPa, and the time is 30 min.
And when the temperature of the workpiece in the hot isostatic pressing machine is reduced to 600 ℃, the returned gas is uniformly pressurized to normal pressure, and then the temperature is kept for 30min to remove the stress.
And finally, mechanically processing and removing the sheath to obtain the hot isostatic pressing diffusion connecting piece.
The hot isostatic pressing diffusion connecting piece prepared by the embodiment has the advantages of tight interface combination, no micro defects and 480MPa of tensile strength.
Example 2
The embodiment provides a preparation method of the invention, which specifically comprises the following steps:
the method comprises the steps of sequentially and respectively grinding phi 25mm by 20mm pure tungsten with the purity of 99.5 wt%, phi 25mm by 0.25mm nickel foil with the purity of 99.9 wt% and phi 25 by 20L steel with the purity of 2000 mm by 200 meshes, 400 meshes, 600 meshes, 1000 meshes and 2000 meshes of abrasive paper, polishing the polished pure tungsten with diamond particles with the particle size of 2-5 mu m to be in a mirror surface state by water, and sequentially and respectively carrying out ultrasonic cleaning for 15 minutes by alcohol and acetone.
Sequentially loading the cleaned pure tungsten, nickel foil and 316L stainless steel into a 316L stainless steel sheath, and covering the sheath and the sheath with an exhaust tube on a H2And welding a sheathing component in the low-oxygen low-humidity argon atmosphere glove box with O content and O content lower than 10ppm by adopting argon arc welding, wherein the exhaust tube and the sheathing cover are made of 316L stainless steel materials. After welding, the sheath is subjected to leak detection, and the leak rate is less than or equal to 4 multiplied by 10-9Pa·m3/s。
Placing the sheath assembly qualified for leak detection in a muffle furnace, connecting an exhaust pipe on a sheath cover with a high vacuum exhaust system, and performing integral heating and degassing on the sheath assembly at 550 ℃ by using the muffle furnace for 3 hours, wherein the vacuum degree in the process is better than 3 multiplied by 10-3Pa. And heating and clamping the exhaust pipe covered on the sheath for three times from the sheath assembly from near to far.
And performing diffusion connection on the sheathed assembly subjected to heating and clamping in a hot isostatic pressing machine, wherein the hot isostatic pressing temperature is 1350 ℃, the pressure is 150MPa, and the time is 90 min.
And when the temperature of the workpiece in the hot isostatic pressing machine is reduced to 500 ℃, the returned gas is uniformly pressurized to normal pressure, and then the temperature is kept for 30min to remove the stress.
And finally, mechanically processing and removing the sheath to obtain the hot isostatic pressing diffusion connecting piece.
The hot isostatic pressing diffusion connecting piece prepared in the embodiment has the advantages of tight interface combination, no micro defects and 426MPa of tensile strength.
Example 3
The embodiment provides a preparation method of the invention, which specifically comprises the following steps:
the method comprises the steps of sequentially and respectively grinding phi 25 multiplied by 20mm pure tungsten with the purity of 99.5 wt%, phi 25 multiplied by 0.25mm copper foil with the purity of 99.9 wt%, phi 30 multiplied by 0.25mm nickel foil with the purity of 99.9 wt% and phi 25 multiplied by 20L 316 steel with the purity of phi 25 multiplied by 20 meshes, 400 meshes, 600 meshes, 1000 meshes and 2000 meshes of sand paper, polishing the sand paper to a mirror surface state by diamond particles with the particle size of 2-5μm in water, and then sequentially and respectively ultrasonically cleaning the sand paper by alcohol and acetone for 20 minutes.
Sequentially loading cleaned pure tungsten, copper foil, nickel foil and 316L stainless steel into a 304 stainless steel sheath, and welding the sheath and a sheath cover with an exhaust tube into a sheath assembly in a high vacuum chamber by adopting electron beams, wherein the vacuum degree is superior to 4 multiplied by 10-3Pa. Wherein the exhaust tube and the sheath cover are both made of 304 stainless steel materials. After welding, the sheath is subjected to leak detection with the leak rate less than or equal to 3 multiplied by 10-9Pa·m3/s。
Placing the sheath assembly qualified for leak detection in a muffle furnace, and covering the sheath with an exhaust tube and a high vacuumThe air pumping system is connected, a muffle furnace is adopted to carry out integral heating degassing on the sheath assembly at the temperature of 600 ℃, the heating degassing is carried out for 2 hours, and the vacuum degree in the process is better than 3 multiplied by 10-3Pa. And heating and clamping the exhaust pipe covered on the sheath for three times from the sheath assembly from near to far.
And performing diffusion bonding on the heated and clamped product in a hot isostatic pressing machine, wherein the hot isostatic pressing temperature is 1050 ℃, the pressure is 155MPa, and the time is 60 min.
And when the temperature of the workpiece in the hot isostatic pressing machine is reduced to 550 ℃, the returned gas is uniformly pressurized to normal pressure, and then the temperature is kept for 30min to remove the stress.
And finally, mechanically processing and removing the sheath to obtain the hot isostatic pressing diffusion connecting piece.
The hot isostatic pressing diffusion connecting piece prepared in the embodiment has the advantages of tight interface combination, no micro defects and tensile strength of 470 MPa.
Example 4
This example is a comparative example
To a purity of 99.5 wt%
Pure tungsten,
The 316L steel is sequentially and respectively ground by 200-mesh, 400-mesh, 600-mesh, 1000-mesh and 2000-mesh sand paper, then polished to a mirror surface state by diamond particle water with the granularity of 2-5 mu m, and then sequentially and respectively ultrasonically cleaned by alcohol and acetone for 20 minutes.
And coating a Ni transition layer of 200 mu m on the surface to be welded of the pure tungsten block by adopting a physical vapor deposition method. And then, sequentially filling the cleaned pure tungsten + Ni transition layer and 316L stainless steel into a 304 stainless steel sheath, and sealing and welding the whole.
And (3) placing the sheath assembly qualified for leak detection in a muffle furnace, connecting an exhaust pipe on the sheath cover with a high-vacuum exhaust system, and performing integral heating and degassing on the sheath assembly at 600 ℃ by using the muffle furnace, wherein the heating and degassing are performed for 2 hours, and the vacuum degree in the process is better than 3 x 10 < -3 > Pa. And heating and clamping the exhaust pipe covered on the sheath for three times from the sheath assembly from near to far.
And performing diffusion bonding on the heated and clamped product in a hot isostatic pressing machine, wherein the hot isostatic pressing temperature is 850 ℃, the pressure is 130MPa, and the time is 3 h.
And removing the sheath at room temperature when the temperature of the workpiece in the hot isostatic pressing machine is high to obtain the hot isostatic pressing diffusion connecting piece, wherein the tensile strength of the connecting piece is 80 MPa.
The interface of the hot isostatic pressing diffusion connecting piece prepared in the embodiment is oxidized, and the surface to be welded is oxidized mainly due to too high temperature during the whole sealing welding of the sheath; the plating layer is made of porous non-compact material, and the adsorbed air is still difficult to be completely desorbed during thermal degassing.
The welding temperature is too low, so that the mutual diffusion of interface elements is insufficient, and the connection strength is low.
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but all the insubstantial modifications or changes made within the spirit and scope of the main design of the present invention, which still solve the technical problems consistent with the present invention, should be included in the scope of the present invention.
Claims (8)
1. A hot isostatic pressing diffusion connection method of tungsten/transition layer/stainless steel is characterized in that pure tungsten, the transition layer and stainless steel are used as raw materials, and hot isostatic pressing treatment, stress relief annealing and de-wrapping are carried out after wrapping treatment, so that a hot isostatic pressing diffusion connection piece can be obtained; the method comprises the following steps:
step 1, assembling: sequentially filling pure tungsten, the transition layer and the stainless steel into a sheath;
step 2, welding: welding the sheath assembled in the step 1 with a sheath cover with an exhaust tube to manufacture a sheath assembly;
and step 3, leak detection: detecting leakage of the sheath assembly prepared in the step 2;
step 4, thermal degassing: placing the sheath assembly qualified in the leak detection in the step 3 into a muffle furnace for thermal degassing;
and step 5, sealing: heating and clamping the exhaust pipe on the sheath assembly after the step 4;
step 6, hot isostatic pressing connection: placing the sheath assembly processed in the step 5 in a hot isostatic pressing machine, and performing diffusion connection on tungsten steel sealed in the sheath;
step 7, stress relief annealing: when the temperature of the workpiece in the hot isostatic pressing machine is reduced to 500-600 ℃, the return gas is uniformly pressurized to normal pressure, and then the heat is preserved and the stress is removed for annealing;
step 8, removing the sheath: turning the sheath assembly annealed in the step 7 to remove sheath materials to obtain the hot isostatic pressing diffusion connecting piece;
the transition layer is selected from one of single transition layers of copper foil, nickel foil and titanium foil, or is a composite transition layer of copper foil and nickel foil;
when the transition layer is a copper foil, the hot isostatic pressing temperature in the step 6 is 1000-1050 ℃;
when the transition layer is a nickel foil, the hot isostatic pressing temperature in the step 6 is 1300-1350 ℃;
when the transition layer is a titanium foil, the hot isostatic pressing temperature in the step 6 is 1250-1350 ℃;
when the transition layer is a copper foil and nickel foil composite layer, the hot isostatic pressing temperature in the step 6 is 950-1050 ℃.
2. The method of hot isostatic pressing diffusion bonding of tungsten/transition layer/stainless steel according to claim 1, further comprising, before assembly, a surface treatment step: grinding and polishing the surfaces to be connected of the pure tungsten, the transition layer and the stainless steel to a mirror surface by using abrasive paper; and after polishing, ultrasonic cleaning is carried out for 10-30 minutes by alcohol and acetone in sequence.
3. The method of claim 1, wherein the pure tungsten is greater than 99.5% by mass tungsten, and the transition layer is greater than 99.8% by mass and has a thickness of 0.1mm to 0.5 mm.
4. The hip diffusion bonding method of W/T/stainless steel as claimed in claim 1, wherein the material of the sheath, sheath cover and exhaust tube is selected from any one of 08F iron sheet, 1Cr18Ni9Ti steel and 316L stainless steel.
5. The method of claim 1, wherein the welding in step 2 is argon arc welding in a low oxygen and low humidity argon shielded glove box; or electron beam welding in a high vacuum chamber.
6. The HIP method of claim 5, wherein step 2 is protection of H inside a glove box during argon arc welding2Both the O content and the O content are lower than 10 ppm; step 2 is that when the electron beam welding is carried out, the vacuum degree in the high vacuum chamber is more than 4 multiplied by 10-3Pa。
7. The method of claim 1, wherein the step of increasing the temperature is performed after the initial pressure is increased to 50MPa to 60 MPa; the heat preservation time is 30min to 120min, and the hot isostatic pressure is 130MPa to 160 MPa.
8. The method of claim 1, wherein in step 7, the annealing for stress relief is performed by holding the temperature for 30min after the return gas is pressurized to normal pressure.
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