CN113909801A - Preparation method of low-activation steel and tungsten all-solid-solution joint - Google Patents
Preparation method of low-activation steel and tungsten all-solid-solution joint Download PDFInfo
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- CN113909801A CN113909801A CN202010650438.XA CN202010650438A CN113909801A CN 113909801 A CN113909801 A CN 113909801A CN 202010650438 A CN202010650438 A CN 202010650438A CN 113909801 A CN113909801 A CN 113909801A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
Abstract
The invention belongs to a connection method, and particularly relates to a preparation method of a low-activation steel and tungsten all-solid-solution joint. It includes: the method comprises the following steps: determining a transition layer material; determining a transition layer material and welding a structure position according to the properties of the base material and the transition layer material; step two: polishing and cleaning; polishing and ultrasonically cleaning the transition layer material and the base material, and performing metal deposition on the surface of the base material; step three: cleaning and assembling; polishing, ultrasonically cleaning and air-drying a parent material tungsten alloy, assembling a vanadium foil strip, a low-activation steel sample subjected to magnetron sputtering and the tungsten alloy from top to bottom according to the sequence of the tungsten alloy/the vanadium foil strip/the chromium coating/the low-activation steel by adopting a tool, and placing the assembled sample in a vacuum hot-pressing furnace; step four: vacuum hot-pressing sintering; and C, carrying out vacuum hot-pressing sintering on the product obtained in the step three. The invention has the following remarkable effects: solving the difference of thermal expansion coefficients between tungsten and low activation steel; the formation of intermetallic compounds between tungsten and low activation steel is avoided.
Description
Technical Field
The invention belongs to a connection method, and particularly relates to a preparation method of a low-activation steel and tungsten all-solid-solution joint.
Background
The plasma-facing components of future fusion reactors are typically composed of plasma-facing materials and heat sink materials or structural materials, applied to the diverters and first walls of the device, subject to high flux plasma and neutron irradiation at 14MeV and significant thermal loads. In the concept design of the helium cold divertor, tungsten is selected as the first choice for the plasma-oriented material due to the advantages of low activity, high melting point, high thermal conductivity, low vapor pressure, low physical sputtering rate, low tritium retention and the like; the low activation steel is used as a structural material, and the plasma-facing component formed by the two components plays a role in discharging heat flow from plasma and helium ash and impurity particles generated by fusion reaction, reducing pollution to central plasma, maintaining a good fusion vacuum environment and the like. If these particles and heat flux are not removed in time, the concentration of plasma and the efficiency of fusion reaction will be reduced, resulting in energy loss of plasma, and in severe cases, fusion devices will be damaged, thus requiring tungsten alloy and low activation steel for good metallurgical gold bonding facing plasma components.
The main joining difficulties of W to RAFM steel are: (1) the melting points (the tungsten melting point is about 3400 ℃, the low-activation steel melting point is about 1500 ℃) have great phase difference, and the direct connection is difficult to realize by common fusion welding; (2) the difference in thermal expansion coefficients is large, for tungsten: 4.5X 10-6K-1The RAFM steel is 12 to 14 multiplied by 10-6K-1When the W and the low-activation steel are directly connected, large residual stress can be generated at a joint, and the welded joint is easily subjected to high thermal stress caused by cyclic heat flux under subsequent working conditions, so that the joint is broken and fails; (3) selecting a solder material: in the future fusion reactor environment, when the divertor runs, the divertor is in the fusion neutron environment, high-neutron active elements such as niobium, nickel, molybdenum, aluminum and copper should be removed, and elements required by low-neutron activation should be selected; therefore, when joining a tungsten alloy to a low activation steel, it is necessary to join themAnd designing a connection interface.
Disclosure of Invention
The invention aims to provide a low activation steel and tungsten all solid solution joint and a connecting method thereof, aiming at the problems of large difference of expansion coefficient and elastic modulus between the tungsten alloy and the metal low activation steel, brittle structure and the like when the tungsten alloy and the metal low activation steel are connected.
The invention is realized by the following steps: a preparation method of a low activation steel and tungsten all solid solution joint comprises the following steps:
the method comprises the following steps: determination of transition layer Material
Determining a transition layer material and welding a structure position according to the properties of the base material and the transition layer material;
step two: polishing and cleaning
Polishing and ultrasonically cleaning the transition layer material and the base material, and performing metal deposition on the surface of the base material;
step three: cleaning and assembling
Polishing, ultrasonically cleaning and air-drying a parent material tungsten alloy, assembling a vanadium foil strip, a low-activation steel sample subjected to magnetron sputtering and the tungsten alloy from top to bottom according to the sequence of the tungsten alloy/the vanadium foil strip/the chromium coating/the low-activation steel by adopting a tool, and placing the assembled sample in a vacuum hot-pressing furnace;
step four: vacuum hot pressing sintering
And C, carrying out vacuum hot-pressing sintering on the product obtained in the step three.
In the method for preparing the low-activation steel and tungsten all-solid-solution joint, the metal deposition on the surface of the base material in the second step is carried out by using a magnetron sputtering method.
The preparation method of the low-activation steel and tungsten all-solid-solution joint is characterized in that the magnetron sputtering mode is that the vacuum degree is 5 x 10-3Carried out under Pa.
The preparation method of the low-activation steel and tungsten full solid solution joint is characterized in that the magnetron sputtering is to deposit and generate a chromium coating or an iron coating on the surface of the parent metal.
The method for preparing the low activation steel and tungsten full solid solution joint is characterized in that the base materials are tungsten alloy and low activation steel, the thermal expansion coefficient of the transition layer material is between the thermal expansion coefficients of the two base materials, and the structural position is tungsten alloy/vanadium alloy/chromium coating/low activation steel or tungsten alloy/vanadium alloy/iron coating/low activation steel.
The preparation method of the low-activation steel and tungsten all-solid-solution joint is characterized in that the thermal expansion coefficient of the transition layer material is between the thermal expansion coefficients of the two base materials, and the gradient of the thermal expansion coefficient of the transition layer material and the thermal expansion coefficient of the base materials is excessive.
The preparation method of the low activation steel and tungsten full solid solution joint is characterized in that the vacuum hot pressing sintering comprises the following sintering parameters of heating rate of 10-20 ℃/min and vacuum degree of less than 5 multiplied by 10-3Pa, sintering temperature of 700-: 0.5-2 h, and the pressure is 100 Mpa.
The preparation method of the low-activation steel and tungsten all-solid-solution joint is characterized in that after sintering is finished, the joint is cooled to room temperature at a temperature of less than 5 ℃/min.
The method for preparing the low-activation steel and tungsten full solid solution joint is characterized in that the purity of the chromium target and the vanadium alloy foil strip is 99.99%.
The preparation method of the low activation steel and tungsten all-solid-solution joint is characterized in that the thickness of the vanadium alloy foil strip is selected to be 1mm-2 mm.
The preparation method of the low-activation steel and tungsten full solid solution joint is characterized in that the thickness of the chromium and iron coating deposited on the low-activation steel by magnetron sputtering is 5-15 mu m.
The invention has the following remarkable effects: the method can solve the problem of the difference of the thermal expansion coefficients of the tungsten and the low-activation steel, avoid the generation of intermetallic compounds between the tungsten and the low-activation steel, and realize good combination of the tungsten and the low-activation steel through solid solution structures. In the invention, vanadium is used as an intermediate transition layer material, in the reaction process, tungsten and vanadium can realize complete solid solution, vanadium and chromium, vanadium and iron, iron and low-activation steel, and chromium and low-activation steel can also realize larger solid solution, a solid solution form connection interface is formed at a certain temperature, time and pressure, firm metallurgical bonding is obtained through process optimization, and the method can be used for the research requirement of the diffusion connection technology of tungsten and low-activation steel in plasma materials of a fusion reactor. Meanwhile, the invention also provides a product prepared by the method and application of the product as a plasma-oriented component.
Detailed Description
The present invention will be specifically described with reference to examples.
Example 1
1) A hot-pressing connection method for obtaining a low-activation steel and tungsten alloy full solid solution joint comprises a base material to be welded and a transition layer material, wherein the base material is a tungsten alloy and a low-activation steel,
2) the screening of the middle layer needs to meet three conditions, and the transition layer material and the main elements of the parent metal to be welded have higher solid solubility; considering that in the future fusion reactor environment, when the divertor runs in the fusion neutron environment, high-neutron active elements such as niobium, nickel, molybdenum, aluminum and copper should be eliminated, and elements required by low-neutron activation should be selected; considering that the base material expansion coefficient difference is large, the tungsten alloy comprises the following components: 4.5X 10-6K-1The low activation steel is 12 to 14 x 10-6K-1The thermal expansion coefficient of W at room temperature is only 0.4 of that of the low activation steel, and the thermal expansion coefficient of the selected transition layer material is between the two, preferably presenting gradient transition; finally, vanadium and chromium are selected as transition layer materials; the selected welding structure position is tungsten alloy/vanadium foil strip/chromium coating/low activation steel;
3) preparation of transition layer materials
Polishing and ultrasonically cleaning a vanadium alloy foil strip as a transition layer material, a chromium target and parent metal low-activation steel to be subjected to magnetron sputtering, and putting the chromium target into a magnetron sputtering device; depositing chromium coatings with the thicknesses of 5 microns, 10 microns and 15 microns on the surface of the low-activation steel by adopting a magnetron sputtering method, wherein the vacuum degree of the chromium coatings reaches 5 multiplied by 10-3Pa; carrying out vacuum packaging on the vanadium foil strip and the low-activation steel sample after the magnetron sputtering is finished;
4) cleaning and assembling parts to be welded
Polishing, ultrasonically cleaning and air-drying a parent material tungsten alloy, assembling a vanadium foil strip and a low-activation steel sample after magnetron sputtering is finished and the tungsten alloy into the sample from top to bottom according to the sequence of the tungsten alloy/the vanadium foil strip/a chromium coating/the low-activation steel by adopting a tool, and placing the sample into a vacuum hot-pressing furnace;
5) vacuum hot pressing sintering
Heating rate of 10-20 deg.C/min, vacuum degree of less than 5 × 10-3Pa, sintering temperature of 700 ℃, and heat preservation time of: 1h, selecting the pressure to be 100 MPa. After sintering, cooling to room temperature at a speed of less than 5 ℃/min to form a compact connecting joint; and (5) sintering the welded part, and taking out the sample.
6) And performing X-ray diffraction and microstructure analysis on the sintered sample interface, and knowing that the interface layer is generated in the series of samples through phase identification and microstructure analysis results.
Example 2
1) A hot-pressing connection method for obtaining a low activation steel and tungsten alloy full solid solution joint comprises a base material and a transition layer material to be welded, wherein the base material is a tungsten alloy and the low activation steel, the screening condition of an intermediate layer is not repeated, and a welding structure is directly selected from the group consisting of a tungsten alloy, a vanadium foil, an iron coating and the low activation steel;
2) preparation of transition layer materials
Polishing and ultrasonically cleaning a vanadium alloy foil strip as a transition layer material, a chromium target and parent metal low-activation steel to be subjected to magnetron sputtering, and putting the chromium target into a magnetron sputtering device; depositing iron coatings with the thickness of 5 microns, 10 microns and 15 microns on the surface of the low-activation steel by adopting a magnetron sputtering method, wherein the vacuum degree of the iron coatings reaches 5 multiplied by 10-3Pa; carrying out vacuum packaging on the vanadium foil strip and the low-activation steel sample after the magnetron sputtering is finished;
3) cleaning and assembling parts to be welded
4) Polishing, ultrasonically cleaning and air-drying a parent material tungsten alloy, assembling a vanadium foil strip and a low-activation steel sample after magnetron sputtering is finished and the tungsten alloy into the sample from top to bottom according to the sequence of the tungsten alloy/the vanadium foil strip/a chromium coating/the low-activation steel by adopting a tool, and placing the sample into a vacuum hot-pressing furnace;
4) vacuum hot pressing sintering
Heating at a rate of 10-20 deg.C/min, and vacuum degree of less than 5 x 10-3Pa, sintering temperature of 700 ℃, and heat preservation time of: 1h, selecting the pressure to be 100 MPa. After sintering, cooling to room temperature at a speed of less than 5 ℃/min to form a compact connecting joint; and (5) sintering the welded part, and taking out the sample.
5) And performing X-ray diffraction and microstructure analysis on the sintered sample interface, and knowing that the interface layer is generated in the series of samples through phase identification and microstructure analysis results.
The invention can obtain the high-strength joint structure of the all solid solution interface, and effectively solves the problem that the interface is easy to crack caused by the brittle structure of the low-activation steel and the tungsten alloy in the connecting process. In the invention, the concentrations of chromium and vanadium are respectively distributed in a gradient way towards two sides of the low-activation steel and the tungsten alloy, and the transition layer can form good bonding strength with the matrix. The invention can meet the requirement of a fusion reactor for plasma component research, and has important significance for component development.
Claims (11)
1. A preparation method of a low-activation steel and tungsten all-solid-solution joint is characterized by comprising the following steps of:
the method comprises the following steps: determination of transition layer Material
Determining a transition layer material and welding a structure position according to the properties of the base material and the transition layer material;
step two: polishing and cleaning
Polishing and ultrasonically cleaning the transition layer material and the base material, and performing metal deposition on the surface of the base material;
step three: cleaning and assembling
Polishing, ultrasonically cleaning and air-drying a parent material tungsten alloy, assembling a vanadium foil strip, a low-activation steel sample subjected to magnetron sputtering and the tungsten alloy from top to bottom according to the sequence of the tungsten alloy/the vanadium foil strip/the chromium coating/the low-activation steel by adopting a tool, and placing the assembled sample in a vacuum hot-pressing furnace;
step four: vacuum hot pressing sintering
And C, carrying out vacuum hot-pressing sintering on the product obtained in the step three.
2. The method of making a low activation steel and tungsten all solid solution joint as claimed in claim 1, wherein: and in the second step, the metal deposition on the surface of the base material is carried out by using a magnetron sputtering mode.
3. The method of making a low activation steel and tungsten all solid solution joint as claimed in claim 2, wherein: the magnetron sputtering method is carried out under the vacuum degree of 5 multiplied by 10-3Carried out under Pa.
4. A method of making a low activation steel and tungsten all solid solution joint as claimed in claim 3 wherein: the magnetron sputtering is to deposit and generate a chromium coating or an iron coating on the surface of the base material.
5. The method of making a low activation steel and tungsten all solid solution joint as claimed in claim 4, wherein: the base materials are tungsten alloy and low-activation steel, the thermal expansion coefficient of the transition layer material is between the thermal expansion coefficients of the two base materials, and the structural position is tungsten alloy/vanadium alloy/chromium coating/low-activation steel or tungsten alloy/vanadium alloy/iron coating/low-activation steel.
6. The method of making a low activation steel and tungsten all solid solution joint as claimed in claim 5, wherein: the thermal expansion coefficient of the transition layer material is between the thermal expansion coefficients of the two base materials, and the gradient of the thermal expansion coefficient, the thermal expansion coefficient of the two base materials is excessive.
7. The method of making a low activation steel and tungsten all solid solution joint as claimed in claim 5, wherein: the vacuum hot-pressing sintering refers to sintering parameters that the heating rate is 10-20 ℃/min, and the vacuum degree is less than 5 multiplied by 10-3Pa, sintering temperature of 700-: 0.5-2 h, and the pressure is 100 Mpa.
8. The method of making a low activation steel and tungsten all solid solution joint as claimed in claim 7, wherein: after sintering, cooling to room temperature at a temperature of less than 5 ℃/min.
9. The method of making a low activation steel and tungsten all solid solution joint as claimed in claim 8, wherein: the purity of the chromium target and the vanadium alloy foil strip was 99.99%.
10. The method of making a low activation steel and tungsten all solid solution joint as claimed in claim 9, wherein: the thickness of the vanadium alloy foil strip is selected to be 1mm-2 mm.
11. The method of making a low activation steel and tungsten all solid solution joint as claimed in claim 10, wherein: the thickness of the chromium and iron coating deposited by magnetron sputtering on the low-activation steel is 5-15 mu m.
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Cited By (2)
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| CN115178852A (en) * | 2022-07-25 | 2022-10-14 | 合肥工业大学 | Diffusion bonding method for connecting tungsten and stainless steel |
| CN115194146A (en) * | 2022-07-22 | 2022-10-18 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Functional gradient layer material suitable for fusion reactor tungsten and steel connection |
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