CN112496518B - Diffusion bonding method of tungsten and low-activation steel - Google Patents
Diffusion bonding method of tungsten and low-activation steel Download PDFInfo
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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
- B23K20/16—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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B23K20/227—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 with ferrous layer
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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
- B23K20/24—Preliminary treatment
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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
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- B23K2103/18—Dissimilar materials
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Abstract
The invention belongs to the field of metal diffusion welding, and particularly relates to a diffusion bonding method of tungsten and low-activation steel, which takes soft low-activation pure vanadium (or pure titanium) and pure iron as composite intermediate layers, combines the composite intermediate layers according to the structure of tungsten/vanadium (or titanium)/iron/low-activation steel, and adopts vacuum hot pressing or hot isostatic pressing to perform diffusion bonding on the combination, wherein the diffusion bonding temperature is controlled to be 700-1000 ℃, and the diffusion bonding time is controlled to be 0.5-4 hours. According to the invention, the brittle reaction layer is controlled between the soft intermediate layers to form a hard/soft/hard interface structure, and the interface stress can be sufficiently slowly released through the plastic deformation or viscoplastic deformation of the soft intermediate layers, so that the initiation and expansion of cracks in the brittle tungsten and the reaction layer are inhibited, and the prepared tungsten/low-activation steel joint has high connection strength, good plasticity and excellent thermal fatigue resistance.
Description
Technical Field
The invention belongs to the field of metal diffusion welding, and particularly relates to a diffusion bonding method of tungsten and low-activation steel.
Background
The plasma facing component is one of the most critical components in the thermonuclear fusion reactor, and the plasma facing component directly faces billions of high-temperature plasmas and needs to bear extremely high thermal load and irradiation of high-energy fusion neutrons, so that the plasma facing component has good thermal fatigue resistance and neutron irradiation resistance. The plasma-facing component is typically composed of a plasma-facing material and a structural material (or heat sink material). Tungsten and its alloys have the advantages of high melting point, high thermal conductivity, low vapor pressure and low sputter corrosion rate, and are considered as the most likely fully-used plasma-facing materials in future tokamak fusion reactors; the low-activation ferrite/martensite steel (RAFM steel) becomes a candidate structural material (or heat sink material) with the advantages of good thermal-mechanical properties, low radiation swelling rate, neutron radiation helium embrittlement resistance and the like, and the reliable connection of the two is one of the key technologies for preparing high-performance plasma facing components. However, the physical properties of tungsten and low activation steel are very different, especially the melting point, and the traditional fusion welding is difficult to realize the connection of the two. The solid diffusion bonding technology is a welding method which ensures atoms on the surface layer of a material to be welded to mutually diffuse to form firm metallurgical bonding only by generating close contact through microscopic local plastic deformation on the surface of the connecting material under the condition that the material to be welded keeps a solid phase state unchanged, has the advantages of low bonding temperature, small influence on the structure and performance of a base metal and the like, and is one of hot research directions of dissimilar metal bonding of tungsten and low-activation steel at present.
Since the difference between the thermal expansion coefficients of tungsten and low activation steel is large, for example, the thermal expansion coefficient of tungsten is 4.5X 10 at 20 deg.C-6K-1The low activation steel has a thermal expansion coefficient of 12 to 14 x 10-6K-1The high residual stresses at the joint interface during cooling to room temperature after welding is achieved in a tungsten/low activation steel joint, which can significantly reduce the room temperature strength and plasticity of the joint and can even lead to joint failure. In addition, the difference in the coefficient of thermal expansion of tungsten/low activation steel under cyclic thermal loading can also result in cyclic high thermal stresses at the joint interface, which can easily lead to crack initiation and propagation, which can significantly reduce the thermal fatigue life of the component.
For this reason, the soft pure metal is usually added as a welding intermediate layer of tungsten and low activation steel to slowly release the interfacial stress between them, so as to improve the joint plasticity and thermal fatigue resistance of the joint. The fusion reactor neutron irradiation environment requires that the soft intermediate layer is low-activation pure metal, which greatly limits the selection range of the intermediate layer, and the intermediate layer meeting the requirements only contains vanadium (V), titanium (Ti), iron (Fe) and zirconium (Zr).
Currently, tungsten/low activation steel joints with certain joint strength and plasticity have been obtained with these four intermediate layers, but there are still disadvantages: the intermediate layer reacts with the base material during the diffusion process to form a brittle reaction layer. Vanadium and titanium do not react with tungsten but form a brittle reaction layer with low activation steel, iron does not react with low activation steel but forms a reaction layer with tungsten, and zirconium forms a reaction layer with both tungsten and low activation steel. The reaction layer is usually in a hard brittle phase, and the base material tungsten and the low activation steel have higher strength, so that the thermal stress between the reaction layer and the base material is difficult to release, and cracks are easy to initiate and propagate from the base material, which reduces the joint connection strength and plasticity, and particularly reduces the interface thermal fatigue resistance. In addition, during the postweld heat treatment of the joint and the high-temperature operation of the fusion reactor, the thickness of a reaction layer is further increased, and the connection performance of the joint is further reduced.
Therefore, it is desired to develop a diffusion bonding method of tungsten and low activation steel, which can improve joint bonding strength, plasticity, and thermal fatigue resistance.
Disclosure of Invention
The invention aims to provide a diffusion bonding method of tungsten and low activation steel, which can obtain a tungsten/low activation steel joint with high bonding strength, plasticity and thermal fatigue resistance.
The technical scheme for realizing the purpose of the invention is as follows: a diffusion bonding method of tungsten and low activation steel adopts pure vanadium and pure iron as a composite intermediate layer to prepare and obtain a tungsten/low activation steel joint with a combination mode of tungsten/pure vanadium/pure iron/low activation steel; or pure titanium and pure iron are used as the composite intermediate layer to prepare the tungsten/low-activation steel joint which has the combination mode of tungsten/pure titanium/pure iron/low-activation steel.
Furthermore, the thickness of the pure vanadium or the pure titanium is 0.1mm-0.5mm, and the thickness of the pure iron is 0.3mm-0.5 mm.
Furthermore, the thickness of the plating layer of pure vanadium or pure titanium is 10-100 μm, and the thickness of pure iron is 0.5-1 mm.
Further, when the thickness of pure vanadium or pure titanium is 0.1mm-0.5mm and the thickness of pure iron is 0.3mm-0.5mm, the diffusion bonding method comprises the following steps:
1) carrying out softening annealing treatment on pure vanadium or pure titanium and pure iron;
2) polishing the surfaces to be welded of tungsten, low-activation steel, pure vanadium or titanium and pure iron to be bright, wherein the surface roughness Ra is less than or equal to 3.2 mu m;
3) pickling the surfaces to be welded of tungsten, low-activation steel, pure vanadium or pure titanium and pure iron;
4) carrying out ultrasonic cleaning on tungsten, low-activation steel, pure vanadium or pure titanium and pure iron;
5) putting tungsten, low-activation steel, pure vanadium or pure titanium and pure iron into a vacuum furnace for vacuum baking and degassing;
6) combining the materials according to the sequence of tungsten/pure vanadium/pure iron/low-activation steel or tungsten/pure titanium/pure iron/low-activation steel, then placing the combination into a mould, and carrying out vacuum hot-pressing diffusion connection or vacuum sealing in a sheath for carrying out hot isostatic pressing diffusion connection to obtain the tungsten/low-activation steel joint.
Further, when the thickness of the plating layer of pure vanadium or pure titanium is 10 μm to 100 μm and the thickness of pure iron is 0.5mm to 1mm, the diffusion bonding method comprises the steps of:
1) carrying out softening annealing treatment on the pure iron;
2) polishing the surfaces to be welded of tungsten, low-activation steel and pure iron to be bright, wherein the surface roughness Ra is less than or equal to 3.2 mu m;
3) pickling the surfaces to be welded of tungsten, low-activation steel and pure iron;
4) carrying out ultrasonic cleaning on tungsten, low-activation steel and pure iron;
5) putting tungsten, low-activation steel and pure iron into a vacuum furnace for vacuum baking and degassing;
6) plating a pure vanadium or pure titanium coating on the surface to be welded of the tungsten by magnetron sputtering;
7) combining the materials according to the sequence of tungsten/pure vanadium/pure iron/low-activation steel or tungsten/pure titanium/pure iron/low-activation steel, then placing the combination into a mould, and carrying out vacuum hot-pressing diffusion connection or vacuum sealing in a sheath for carrying out hot isostatic pressing diffusion connection to obtain the tungsten/low-activation steel joint.
Further, the temperature of the vacuum hot-pressing diffusion connection is 800--3Pa。
Furthermore, the temperature of the hot isostatic pressing diffusion connection is 700-1000 ℃, the pressure is 60-180MPa, and the time is 0.5-4 h.
Further, the solvent for acid washing is dilute hydrochloric acid.
Further, solvents for ultrasonic cleaning are acetone and alcohol.
Further, the temperature of vacuum baking degassing is 300 ℃, and the vacuum degree is less than or equal to 1 multiplied by 10-3Pa, time 120 min.
The invention has the beneficial technical effects that: according to the diffusion bonding method of the tungsten and the low-activation steel, the brittle reaction layer is controlled between the soft intermediate layers, namely between vanadium and iron or between titanium and iron, so that a hard/soft/hard interface structure is formed, interface stress can be sufficiently slowly released through plastic deformation or viscoplastic deformation of the soft intermediate layers, high interface stress introduced into the brittle reaction layer is avoided, initiation and expansion of cracks in the brittle tungsten and the reaction layer are inhibited, and the prepared tungsten/low-activation steel joint can have high bonding strength, good plasticity and excellent thermal fatigue resistance.
Drawings
Fig. 1 is a schematic structural diagram of a tungsten and low activation steel joint prepared by a diffusion bonding method of tungsten and low activation steel provided by the invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
The preparation of tungsten/low activation steel joints was carried out with pure vanadium or pure titanium as foil material with a thickness of 0.1-0.5mm, see in particular examples 1-3.
Example 1 preparation of a tungsten/vanadium/iron/Low activation Steel Joint
1) Processing pure tungsten, pure vanadium, pure iron and low activation steel into the sizes of 30mm multiplied by 3mm, 30mm multiplied by 0.5mm, 30mm multiplied by 0.3mm and 30mm multiplied by 30mm respectively;
2) carrying out vacuum softening annealing treatment on the pure vanadium foil and the pure iron foil, wherein the annealing processes are respectively 700 ℃ heat preservation for 30min and 600 ℃ heat preservation for 60min, and the vacuum degrees are respectively less than or equal to 1 multiplied by 10-3Pa；
3) Polishing the surfaces to be welded of pure tungsten, low-activation steel, pure vanadium and pure iron by using SiC sand paper to be bright, wherein the surface roughness Ra is less than or equal to 3.2 mu m;
4) carrying out acid cleaning on surfaces to be welded of pure tungsten, low-activation steel, pure vanadium foil and pure iron foil by using dilute hydrochloric acid with volume fraction of 5% to remove residual oxides on the surfaces;
5) sequentially putting the acid-washed pure tungsten, low-activation steel, pure vanadium foil and pure iron foil into acetone and alcohol for ultrasonic cleaning, and respectively performing ultrasonic cleaning for 20 min;
6) the cleaned pure tungsten, low activation steel, pure vanadium foil and pure iron foil are put into a vacuum furnace for vacuum baking degassing, and the vacuum degree is less than or equal to 1 multiplied by 10 at 300 DEG C-3Keeping the temperature for 120min under the condition of Pa;
7) combining the materials according to the sequence of tungsten/vanadium/iron/low-activation steel, then placing the combination in a 304 stainless steel sheath, carrying out vacuum exhaust on the sheath for 6 hours, then clamping and sealing by adopting TIG welding to form a sheath sealing body;
8) placing the sheath sealing body into a hot isostatic pressing furnace for hot isostatic pressing diffusion connection, wherein the hot isostatic pressing temperature is 700 ℃, the pressure is 180MPa, the heat preservation time is 4h, and the temperature rise and fall speed is 10 ℃/min;
9) and removing the 304 stainless steel sheath by using a milling machine to obtain the tungsten/low-activation steel joint.
Example 2 preparation of a tungsten/titanium/iron/Low activation Steel Joint
1) Processing pure tungsten, pure titanium, pure iron and low activation steel into the dimensions of 30mm × 30mm × 3mm, 30mm × 30mm × 0.1mm, 30mm × 30mm × 0.4mm and 30mm × 30mm × 30mm × 30mm, respectively;
2) carrying out vacuum softening annealing treatment on pure titanium foil and pure iron foil, wherein the annealing processes are respectively 700 ℃ heat preservation for 30min and 600 ℃ heat preservation for 60min, and the vacuum degrees are respectively less than or equal to 1 multiplied by 10-3Pa；
3) Polishing the surfaces to be welded of pure tungsten, low-activation steel, pure titanium and pure iron by using SiC sand paper to be bright, wherein the surface roughness Ra is less than or equal to 3.2 mu m;
4) carrying out acid cleaning on surfaces to be welded of pure tungsten, low-activation steel, pure titanium foil and pure iron foil by using dilute hydrochloric acid with volume fraction of 5% to remove residual oxides on the surfaces;
5) sequentially putting the acid-washed pure tungsten, low-activation steel, pure titanium foil and pure iron foil into acetone and alcohol for ultrasonic cleaning, and respectively performing ultrasonic cleaning for 20 min;
6) the cleaned pure tungsten, low-activation steel, pure titanium foil and pure iron foil are put into a vacuum furnace for vacuum baking degassing, and the vacuum degree is less than or equal to 1 multiplied by 10 at 300 DEG C-3Keeping the temperature for 120min under the condition of Pa;
7) the materials after degassing are combined according to the sequence of tungsten/vanadium/iron/low activation steel, then the combination is placed in a vacuum hot pressing furnace mould for vacuum hot pressing diffusion connection, the vacuum hot pressing temperature is 850 ℃, the pressure is 30MPa, the heat preservation time is 3h, the temperature rise and fall rate is 10 ℃/min, the vacuum degree is less than or equal to 1 multiplied by 10-3Pa；
8) And removing the die after the vacuum hot pressing is finished, and obtaining the tungsten/low-activation steel joint.
Example 3 preparation of a tungsten/vanadium/iron/Low activation Steel Joint
1) Processing pure tungsten, pure vanadium, pure iron and low activation steel into the sizes of 30mm multiplied by 3mm, 30mm multiplied by 0.3mm, 30mm multiplied by 0.5mm and 30mm multiplied by 30mm respectively;
2) carrying out vacuum softening annealing treatment on the pure vanadium foil and the pure iron foil, wherein the annealing processes are respectively 700 ℃ heat preservation for 30min and 600 ℃ heat preservation for 60min, and the vacuum degrees are respectively less than or equal to 1 multiplied by 10-3Pa；
3) Polishing the surfaces to be welded of pure tungsten, low-activation steel, pure vanadium and pure iron by using SiC sand paper to be bright, wherein the surface roughness Ra is less than or equal to 3.2 mu m;
4) carrying out acid cleaning on surfaces to be welded of pure tungsten, low-activation steel, pure vanadium foil and pure iron foil by using dilute hydrochloric acid with volume fraction of 5% to remove residual oxides on the surfaces;
5) sequentially putting the acid-washed pure tungsten, low-activation steel, pure vanadium foil and pure iron foil into acetone and alcohol for ultrasonic cleaning, and respectively performing ultrasonic cleaning for 20 min;
6) the cleaned pure tungsten, low activation steel, pure vanadium foil and pure iron foil are put into a vacuum furnace for vacuum baking degassing, and the vacuum degree is less than or equal to 1 multiplied by 10 at 300 DEG C-3Keeping the temperature for 120min under the condition of Pa;
7) the materials after degassing are combined according to the sequence of tungsten/vanadium/iron/low activation steel, then the combination is placed in a vacuum hot pressing furnace mould for diffusion connection, the vacuum hot pressing temperature is 1000 ℃, the pressure is 10MPa, the heat preservation time is 1h, the temperature rise and fall rate is 10 ℃/min, the vacuum degree is less than or equal to 1 multiplied by 10-3Pa；
8) And removing the die after the vacuum hot pressing is finished, and obtaining the tungsten/low-activation steel joint.
The preparation of tungsten/low activation steel joints was carried out with pure vanadium or pure titanium as coating material with a thickness of 10-100 μm, see in particular examples 4-6.
EXAMPLE 4 preparation of tungsten/titanium/iron/Low activation Steel joints
1) Processing pure tungsten, pure iron and low-activation steel into the dimensions of 20mm multiplied by 3mm, 20mm multiplied by 1mm and 20mm multiplied by 30mm respectively;
2) carrying out vacuum softening annealing treatment on the pure iron foil, wherein the annealing process is that the temperature is kept for 60min at 600 ℃, and the vacuum degree is less than or equal to 1 multiplied by 10-3Pa；
3) Polishing the surfaces to be welded of the pure tungsten, the low-activation steel and the pure iron by using SiC sand paper to be bright, wherein the surface roughness Ra is less than or equal to 3.2 mu m;
4) carrying out acid cleaning on surfaces to be welded of pure tungsten, low-activation steel and pure iron foil by using dilute hydrochloric acid with volume fraction of 5% to remove residual oxides on the surfaces;
5) sequentially putting the acid-washed pure tungsten, low-activation steel and pure iron foil into acetone and alcohol for ultrasonic cleaning, and respectively performing ultrasonic cleaning for 20 min;
6) the cleaned pure tungsten, the low activation steel andplacing the pure iron foil into a vacuum furnace for vacuum baking and degassing, wherein the vacuum degree is less than or equal to 1 multiplied by 10 at 300 DEG C-3Keeping the temperature for 120min under the condition of Pa;
7) plating a titanium coating with the thickness of about 10 mu m on the surface to be welded of the tungsten by adopting magnetron sputtering;
8) combining the materials in the order of tungsten/titanium/iron/low activation steel, and then placing the combination in a vacuum hot pressing furnace mould for diffusion connection, wherein the vacuum hot pressing temperature is 900 ℃, the pressure is 20MPa, and the vacuum degree is less than or equal to 1 multiplied by 10-3Pa, the heat preservation time is 2h, and the heating and cooling rates are both 10 ℃/min;
9) and removing the die after the vacuum hot pressing is finished, and obtaining the tungsten/low-activation steel joint.
Example 5 preparation of tungsten/vanadium/iron/Low activation Steel joints
1) Processing pure tungsten, pure iron and low activation steel into the dimensions of 20mm multiplied by 3mm, 20mm multiplied by 0.5mm and 20mm multiplied by 30mm respectively;
2) carrying out vacuum softening annealing treatment on the pure iron foil, wherein the annealing process is that the temperature is kept for 60min at 600 ℃, and the vacuum degree is less than or equal to 1 multiplied by 10-3Pa；
3) Polishing the surfaces to be welded of the pure tungsten, the low-activation steel and the pure iron by using SiC sand paper to be bright, wherein the surface roughness Ra is less than or equal to 3.2 mu m;
4) carrying out acid cleaning on surfaces to be welded of pure tungsten, low-activation steel and pure iron foil by using dilute hydrochloric acid with volume fraction of 5% to remove residual oxides on the surfaces;
5) sequentially putting the acid-washed pure tungsten, low-activation steel and pure iron foil into acetone and alcohol for ultrasonic cleaning, and respectively performing ultrasonic cleaning for 20 min;
6) the cleaned pure tungsten, low activation steel and pure iron foil are put into a vacuum furnace for vacuum baking degassing, and the vacuum degree is less than or equal to 1 multiplied by 10 at 300 DEG C-3Keeping the temperature for 120min under the condition of Pa;
7) plating a vanadium coating with the thickness of about 50 microns on the surface to be welded of the tungsten by magnetron sputtering;
8) combining the materials according to the sequence of tungsten/vanadium/iron/low-activation steel, then placing the combination in a 304 stainless steel sheath, carrying out vacuum exhaust on the sheath for 6 hours, then clamping and sealing by adopting TIG welding to form a sheath sealing body;
9) placing the sheath sealing body into a hot isostatic pressing furnace for hot isostatic pressing diffusion connection, wherein the hot isostatic pressing temperature is 1000 ℃, the pressure is 60MPa, the heat preservation time is 0.5h, and the temperature rise and fall speed is 10 ℃/min;
10) and removing the 304 stainless steel sheath by using a milling machine to obtain the tungsten/low-activation steel joint.
EXAMPLE 6 preparation of tungsten/titanium/iron/Low activation Steel joints
1) Processing pure tungsten, pure iron and low activation steel into the dimensions of 20mm multiplied by 3mm, 20mm multiplied by 0.7mm and 20mm multiplied by 30mm respectively;
2) carrying out vacuum softening annealing treatment on the pure iron foil, wherein the annealing process is that the temperature is kept for 60min at 600 ℃, and the vacuum degree is less than or equal to 1 multiplied by 10-3Pa；
3) Polishing the surfaces to be welded of the pure tungsten, the low-activation steel and the pure iron by using SiC sand paper to be bright, wherein the surface roughness Ra is less than or equal to 3.2 mu m;
4) carrying out acid cleaning on surfaces to be welded of pure tungsten, low-activation steel and pure iron foil by using dilute hydrochloric acid with volume fraction of 5% to remove residual oxides on the surfaces;
5) sequentially putting the acid-washed pure tungsten, low-activation steel and pure iron foil into acetone and alcohol for ultrasonic cleaning, and respectively performing ultrasonic cleaning for 20 min;
6) the cleaned pure tungsten, low activation steel and pure iron foil are put into a vacuum furnace for vacuum baking degassing, and the vacuum degree is less than or equal to 1 multiplied by 10 at 300 DEG C-3Keeping the temperature for 120min under the condition of Pa;
7) plating a titanium coating with the thickness of about 100 mu m on the surface to be welded of the tungsten by adopting magnetron sputtering;
8) combining the materials according to the sequence of tungsten/titanium/iron/low-activation steel, then placing the combination in a 304 stainless steel sheath, carrying out vacuum exhaust on the sheath for 6 hours, then clamping and sealing by adopting TIG welding to form a sheath sealing body;
9) placing the sheath sealing body into a hot isostatic pressing furnace for hot isostatic pressing diffusion connection, wherein the hot isostatic pressing temperature is 800 ℃, the pressure is 100MPa, the heat preservation time is 3h, and the temperature rise and fall speed is 10 ℃/min;
10) and removing the 304 stainless steel sheath by using a milling machine to obtain the tungsten/low-activation steel joint.
Comparative example 1 preparation of tungsten/vanadium/Low activation Steel Joint
A single-layer pure vanadium of 1mm was used as an intermediate layer, and the tungsten/low activation steel diffusion bonded joint was prepared using the same annealing treatment, surface polishing, acid washing, ultrasonic cleaning, vacuum baking degassing, and hot isostatic pressing diffusion bonding processes and parameters as in example 1.
Comparative example 2 preparation of tungsten/titanium/Low activation Steel Joint
A tungsten/low activation steel diffusion bonded joint was prepared using a 0.5mm single layer of pure titanium as an intermediate layer, using the same annealing treatment, surface polishing, acid cleaning, ultrasonic cleaning, vacuum baking degassing, and vacuum hot pressing diffusion bonding processes and parameters as in example 2.
Comparative example 3 preparation of tungsten/vanadium/Low activation Steel Joint
A single-layer pure vanadium with the thickness of 0.8mm is used as an intermediate layer, and the tungsten/low-activation steel diffusion connection joint is prepared by adopting the same annealing treatment, surface polishing, acid cleaning, ultrasonic cleaning, vacuum baking degassing and vacuum hot-pressing diffusion connection process and parameters as those in the embodiment 3.
Comparative example 4 preparation of a tungsten/iron/Low activation Steel Joint
A tungsten/low activation steel diffusion bonded joint was prepared using a 0.5mm single layer of pure iron as the intermediate layer and using the same annealing treatment, surface polishing, acid cleaning, ultrasonic cleaning, vacuum baking degassing, and hot isostatic pressing diffusion bonding processes and parameters as in example 5.
Example 7
The tungsten and low activation steel joints prepared in examples 1 to 6 and comparative examples 1 to 4 were tested for joint strength and plasticity as indicated by the peak shear strength and peak shear displacement, and the results are shown in table 1.
TABLE 1 results of joint strength and plasticity tests of tungsten/low activation steel joints
The results in table 1 show that the tungsten and low-activation steel joint with the composite intermediate layer prepared by the diffusion bonding method of tungsten and low-activation steel of the invention has obviously improved bonding strength and plasticity compared with the tungsten and low-activation steel joint with a single intermediate layer, and the improvement of interfacial plasticity can obviously improve the interface thermal fatigue resistance and prolong the thermal fatigue life of the component.
The present invention has been described in detail with reference to the drawings and examples, but the present invention is not limited to the examples, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. The prior art can be adopted in the content which is not described in detail in the invention.
Claims (9)
1. The diffusion bonding method of tungsten and low activation steel is characterized in that pure vanadium and pure iron are used as a composite intermediate layer, and a joint of tungsten and low activation steel with a combination mode of tungsten/pure vanadium/pure iron/low activation steel is prepared; or pure titanium and pure iron are adopted as a composite intermediate layer, and the joint of tungsten and low-activation steel with a combination mode of tungsten/pure titanium/pure iron/low-activation steel is prepared; the thickness of the pure vanadium or the pure titanium is 0.1mm-0.5mm, and the thickness of the pure iron is 0.3mm-0.5 mm.
2. The diffusion bonding method of tungsten and low activation steel is characterized in that pure vanadium and pure iron are used as a composite intermediate layer, and a joint of tungsten and low activation steel with a combination mode of tungsten/pure vanadium/pure iron/low activation steel is prepared; or pure titanium and pure iron are adopted as a composite intermediate layer, and the joint of tungsten and low-activation steel with a combination mode of tungsten/pure titanium/pure iron/low-activation steel is prepared; the thickness of the pure vanadium or pure titanium coating is 10-100 μm, and the thickness of the pure iron is 0.5-1 mm.
3. The diffusion bonding method of tungsten and low activation steel according to claim 1, wherein said diffusion bonding method comprises the steps of:
1) carrying out softening annealing treatment on pure vanadium or pure titanium and pure iron;
2) polishing the surfaces to be welded of tungsten, low-activation steel, pure vanadium or titanium and pure iron to be bright, wherein the roughness is less than or equal to 3.2 mu m;
3) pickling the surfaces to be welded of tungsten, low-activation steel, pure vanadium or pure titanium and pure iron;
4) carrying out ultrasonic cleaning on tungsten, low-activation steel, pure vanadium or pure titanium and pure iron;
5) putting tungsten, low-activation steel, pure vanadium or pure titanium and pure iron into a vacuum furnace for vacuum baking and degassing;
6) combining the materials according to the sequence of tungsten/pure vanadium/pure iron/low-activation steel or tungsten/pure titanium/pure iron/low-activation steel, then placing the combination into a mould, and carrying out vacuum hot-pressing diffusion connection or vacuum sealing in a sheath for carrying out hot isostatic pressing diffusion connection to obtain the joint of tungsten and low-activation steel.
4. The diffusion bonding method of tungsten and low activation steel according to claim 2, wherein said diffusion bonding method comprises the steps of:
1) carrying out softening annealing treatment on the pure iron;
2) polishing the surfaces to be welded of tungsten, low-activation steel and pure iron to be bright, wherein the roughness is less than or equal to 3.2 microns;
3) pickling the surfaces to be welded of tungsten, low-activation steel and pure iron;
4) carrying out ultrasonic cleaning on tungsten, low-activation steel and pure iron;
5) putting tungsten, low-activation steel and pure iron into a vacuum furnace for vacuum baking and degassing;
6) plating a pure vanadium or pure titanium coating on the surface to be welded of the tungsten by magnetron sputtering;
7) combining the materials according to the sequence of tungsten/pure vanadium/pure iron/low-activation steel or tungsten/pure titanium/pure iron/low-activation steel, then placing the combination into a mould, and carrying out vacuum hot-pressing diffusion connection or vacuum sealing in a sheath for carrying out hot isostatic pressing diffusion connection to obtain the joint of tungsten and low-activation steel.
5. The diffusion bonding method of tungsten and low activation steel as claimed in claim 3 or 4, wherein the temperature of the vacuum hot-pressing diffusion bonding is 800-1000 ℃, the pressure is 10-30MPa, the time is 1-4h, and the vacuum degree is less than or equal to 1 x 10-3Pa。
6. The method of claim 3 or 4, wherein the hot isostatic pressing diffusion bonding is performed at a temperature of 700 ℃ and 1000 ℃, at a pressure of 60 to 180MPa, and for a time of 0.5 to 4 hours.
7. The method of claim 3 or 4, wherein the acid-washing solvent is dilute hydrochloric acid.
8. The method of claim 3 or 4, wherein the solvents for ultrasonic cleaning are acetone and alcohol.
9. The method for diffusion bonding of tungsten and low activation steel according to claim 3 or 4, wherein the temperature of the vacuum baking degassing is 300 ℃ and the degree of vacuum is less than or equal to 1 x 10-3Pa, time 120 min.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09323190A (en) * | 1996-06-04 | 1997-12-16 | Nippon Steel Corp | Alloy foil for liquid phase diffusion joining of fe base metal enabling joining in oxidizing atmosphere |
| CN105216394A (en) * | 2015-10-30 | 2016-01-06 | 中南大学 | A kind of High Performance W/steel composite material based on high temperature application and preparation method thereof |
| CN105346161A (en) * | 2015-10-30 | 2016-02-24 | 中南大学 | Tungsten/transition layer/steel composite material and low-temperature and low-pressure active diffusion connection preparation method thereof |
| CN105499816A (en) * | 2016-02-02 | 2016-04-20 | 中国科学院等离子体物理研究所 | Manufacturing process suitable for tungsten and steel connection of first wall part of fusion reactor |
| CN108788436A (en) * | 2018-06-05 | 2018-11-13 | 中国科学院合肥物质科学研究院 | A kind of technique connecting fusion reactor material tungsten and steel using the diffusion of hydrogen metal is set |
| CN109396631A (en) * | 2018-11-14 | 2019-03-01 | 中国工程物理研究院材料研究所 | A kind of tungsten/transition zone/stainless steel hot isostatic pressing diffusion connection method |
| CN111347146A (en) * | 2018-12-24 | 2020-06-30 | 核工业西南物理研究院 | Tungsten and heat sink material connector and preparation method thereof |
| CN111347147A (en) * | 2018-12-24 | 2020-06-30 | 核工业西南物理研究院 | Hot isostatic pressing connection method of tungsten and heat sink material |
-
2020
- 2020-11-11 CN CN202011255864.XA patent/CN112496518B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09323190A (en) * | 1996-06-04 | 1997-12-16 | Nippon Steel Corp | Alloy foil for liquid phase diffusion joining of fe base metal enabling joining in oxidizing atmosphere |
| CN105216394A (en) * | 2015-10-30 | 2016-01-06 | 中南大学 | A kind of High Performance W/steel composite material based on high temperature application and preparation method thereof |
| CN105346161A (en) * | 2015-10-30 | 2016-02-24 | 中南大学 | Tungsten/transition layer/steel composite material and low-temperature and low-pressure active diffusion connection preparation method thereof |
| CN105499816A (en) * | 2016-02-02 | 2016-04-20 | 中国科学院等离子体物理研究所 | Manufacturing process suitable for tungsten and steel connection of first wall part of fusion reactor |
| CN108788436A (en) * | 2018-06-05 | 2018-11-13 | 中国科学院合肥物质科学研究院 | A kind of technique connecting fusion reactor material tungsten and steel using the diffusion of hydrogen metal is set |
| CN109396631A (en) * | 2018-11-14 | 2019-03-01 | 中国工程物理研究院材料研究所 | A kind of tungsten/transition zone/stainless steel hot isostatic pressing diffusion connection method |
| CN111347146A (en) * | 2018-12-24 | 2020-06-30 | 核工业西南物理研究院 | Tungsten and heat sink material connector and preparation method thereof |
| CN111347147A (en) * | 2018-12-24 | 2020-06-30 | 核工业西南物理研究院 | Hot isostatic pressing connection method of tungsten and heat sink material |
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