CN113909801B - Preparation method of low-activation steel and tungsten complete solid solution joint - Google Patents
Preparation method of low-activation steel and tungsten complete solid solution joint Download PDFInfo
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- CN113909801B CN113909801B CN202010650438.XA CN202010650438A CN113909801B CN 113909801 B CN113909801 B CN 113909801B CN 202010650438 A CN202010650438 A CN 202010650438A CN 113909801 B CN113909801 B CN 113909801B
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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
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Abstract
The invention belongs to a connecting method, and particularly relates to a preparation method of a low-activation steel and tungsten complete solid solution joint. It comprises the following steps: step one: determining a transition layer material; determining a transition layer material and a welding structure position according to the properties of a base material and the transition layer material; step two: polishing and cleaning; polishing and ultrasonic cleaning the transition layer material and the base material, and carrying out metal deposition on the surface of the base material; step three: cleaning and assembling; polishing and ultrasonically cleaning a base metal tungsten alloy, air-drying, assembling a vanadium foil strip, a magnetron sputtered low-activation steel sample and the tungsten alloy into a sample from top to bottom in the sequence of the tungsten alloy, the vanadium foil strip, the chromium coating and the low-activation steel by adopting a tool, and placing the sample in a vacuum hot-pressing furnace; step four: vacuum hot-pressing sintering; and (3) carrying out vacuum hot-pressing sintering on the product obtained in the step (III). The invention has the remarkable effects that: solving the difference of thermal expansion coefficients between tungsten and low-activation steel; avoiding the formation of intermetallic compounds between tungsten and low activation steel.
Description
Technical Field
The invention belongs to a connecting method, and particularly relates to a preparation method of a low-activation steel and tungsten complete solid solution joint.
Background
The plasma-facing components of future fusion stacks are typically composed of a plasma-facing material and a heat sink material or structural material, applied to the divertor and first wall of the device, subjected to high flux plasma and 14MeV neutron irradiation and significant thermal loading. In the conceptual design of helium cold divertors, tungsten is selected as the first choice for plasma-oriented materials due to its low activity, high melting point, high thermal conductivity, low vapor pressure, low physical sputtering rate, low tritium retention, etc.; the low-activation steel is used as a structural material, and the plasma-facing component formed by the low-activation steel and the low-activation steel plays roles of discharging heat flow from plasma and helium ash and impurity particles generated by fusion reaction, reducing pollution to central plasma, maintaining good fusion vacuum environment and the like. If these particles and heat flux are not removed in time, the concentration of the plasma and the efficiency of fusion reaction will decrease, resulting in energy loss of the plasma, and in severe cases, the fusion device will be damaged, so that tungsten alloy and low activation steel are required to be bonded with metallurgical gold for the plasma-oriented component.
The main difficulties of connection of W to RAFM steel are: (1) The melting points (the melting point of tungsten is about 3400 ℃ and the melting point of low-activation steel is about 1500 ℃) are greatly different, and direct connection is difficult to realize by common fusion welding; (2) a large difference in thermal expansion coefficient, for tungsten: 4.5X10 -6 K -1 RAFM steel is 12-14×10 -6 K -1 The thermal expansion coefficient of W is only 0.4 of that of low-activation steel at room temperature, and the elastic modulus is 2 times of that of the low-activation steel, when the W and the low-activation steel are directly connected, larger residual stress is generated at the joint, and the welded joint is easy to receive the circulating heat flux under the subsequent working condition to generate high heat stress, so that the joint is broken and fails; (3) solder material selection: because the divertor in the future fusion reactor environment is in the fusion neutron environment when in operation, high neutron active elements such as niobium, nickel, molybdenum, aluminum, copper and the like should be removed, and elements with low neutron activation requirement should be selected; therefore, when the tungsten alloy is connected with the low activation steel, the connection interface thereof must be designed.
Disclosure of Invention
The invention aims to provide a low-activation steel and tungsten complete solid solution joint and a connecting method thereof, aiming at the problems of large expansion coefficient and elastic modulus difference between tungsten alloy and metal low-activation steel, brittle tissue and the like when the tungsten alloy and the metal low-activation steel are connected.
The invention is realized in the following way: a method for preparing a low-activation steel and tungsten complete solid solution joint, which comprises the following steps:
step one: determination of transition layer material
Determining a transition layer material and a welding structure position according to the properties of a base material and the transition layer material;
step two: polishing and cleaning
Polishing and ultrasonic cleaning the transition layer material and the base material, and carrying out metal deposition on the surface of the base material;
step three: cleaning and assembly
Polishing and ultrasonically cleaning a base metal tungsten alloy, air-drying, assembling a vanadium foil strip, a magnetron sputtered low-activation steel sample and the tungsten alloy into a sample from top to bottom in the sequence of the tungsten alloy, the vanadium foil strip, the chromium coating and the low-activation steel by adopting a tool, and placing the sample in a vacuum hot-pressing furnace;
step four: vacuum hot-pressing sintering
And (3) carrying out vacuum hot-pressing sintering on the product obtained in the step (III).
The preparation method of the low-activation steel and tungsten complete solid solution joint comprises the step two, wherein the surface metal deposition of the base metal is performed by using a magnetron sputtering mode.
The preparation method of the low-activation steel and tungsten complete solid solution joint comprises the steps of adopting a magnetron sputtering mode, wherein the vacuum degree is 5 multiplied by 10 -3 Under Pa conditions.
The preparation method of the low-activation steel and tungsten complete solid solution joint comprises the step of depositing a chromium coating or an iron coating on the surface of a base material by magnetron sputtering.
The preparation method of the low-activation steel and tungsten complete solid solution joint comprises the steps 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 structure 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 complete solid solution joint is characterized in that the thermal expansion coefficient of the transition layer material is between the thermal expansion coefficients of 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 complete solid solution joint comprises the steps of vacuum hot-press sintering, wherein the sintering parameters are that the heating rate is 10-20 ℃/min, and the vacuum degree is less than 5 multiplied by 10 -3 Pa, sintering temperature is 700-760 ℃, and heat preservation time is as follows: the pressure is selected to be 100Mpa after 0.5-2 h.
The preparation method of the low-activation steel and tungsten complete solid solution joint comprises the steps of cooling to room temperature at a speed of less than 5 ℃ per minute after sintering.
The preparation method of the low-activation steel and tungsten complete solid solution joint comprises the step of preparing a chromium target and vanadium alloy foil strip, wherein the purity of the chromium target and the vanadium alloy foil strip is 99.9%.
The preparation method of the low-activation steel and tungsten complete solid solution joint comprises the step of selecting the thickness of a vanadium alloy foil strip to be 1-2 mm.
The preparation method of the low-activation steel and tungsten complete solid solution joint comprises the step of magnetically controlling the thickness of a chromium and iron coating deposited on the low-activation steel to be 5-15 mu m.
The invention has the remarkable effects that: the invention can not only solve the difference of thermal expansion coefficients between tungsten and low-activation steel, but also avoid generating intermetallic compounds between tungsten and low-activation steel, and realize good combination between tungsten and low-activation steel through solid solution tissues. 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, chromium and low-activation steel can also realize larger solid solution, a solid solution type connecting 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 requirements of diffusion connection technology research of tungsten and low-activation steel in a fusion reactor facing plasma materials. Meanwhile, the invention also provides a product prepared by the method and application of the product as a plasma-oriented component.
Detailed Description
The invention is specifically illustrated below with reference to examples.
Example 1
1) A hot-press connection method for obtaining a low-activation steel and tungsten alloy full solid solution joint comprises a base metal to be welded and a transition layer material, wherein the base metal is tungsten alloy and low-activation steel,
2) The intermediate layer screening needs to meet three conditions, and the transition layer material and the main elements of the parent metal to be welded have larger solid solubility; considering that the divertor in the future fusion reactor environment is in fusion neutron environment when in operation, high neutron active elements such as niobium, nickel, molybdenum, aluminum, copper and the like should be removed, and elements with low neutron activation requirement should be selected; taking into account thatThe difference of the expansion coefficients of the base materials is large, and for tungsten alloy: 4.5X10 -6 K -1 The low-activation steel is 12-14 multiplied by 10 -6 K -1 The thermal expansion coefficient of W is only 0.4 of that of low-activation steel at room temperature, and the thermal expansion coefficient of the selected transition layer material is positioned between the two materials, and gradient transition is preferably presented; finally selecting vanadium and chromium as transition layer materials; the selected welding structure is tungsten alloy/vanadium foil belt/chromium coating/low activation steel;
3) Preparation of transition layer materials
Polishing and ultrasonically cleaning a transition layer material vanadium alloy foil belt, 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; chromium coating with thickness of 5 μm,10 μm and 15 μm is deposited on the surface of low-activation steel by magnetron sputtering method, and vacuum degree reaches 5×10 -3 Pa; vacuum packaging the vanadium foil strip and the low-activation steel sample after magnetron sputtering is completed;
4) Cleaning and assembling of parts to be welded
Polishing and ultrasonically cleaning a base metal tungsten alloy, air-drying, assembling a vanadium foil strip, a low-activation steel sample subjected to magnetron sputtering by adopting a tool, and the tungsten alloy into a sample from top to bottom according to the sequence of the tungsten alloy, the vanadium foil strip, the chromium coating and the low-activation steel, and placing the sample in a vacuum hot-pressing furnace;
5) Vacuum hot-pressing sintering
The heating rate is 10-20deg.C/min, and the vacuum degree is less than 5×10 -3 Pa, sintering temperature is 700 ℃, and heat preservation time is as follows: the pressure was chosen to be 100MPa for 1h. Cooling to room temperature at a speed of less than 5 ℃ per minute after sintering to form a compact connecting joint; and (5) sintering the welding piece, and taking out the sample.
6) X-ray diffraction and microstructure analysis are carried out on the sintered sample interface, and the interface layer is generated in the series of samples according to the phase identification and the microstructure analysis result.
Example 2
1) A hot-press connection method for obtaining a low-activation steel and tungsten alloy complete solid solution joint comprises the steps of welding a parent metal and a transition layer material, wherein the parent metal is tungsten alloy and low-activation steel, the screening condition of an intermediate layer is not repeated here, and a welding structure is directly selected as tungsten alloy/vanadium foil strip/iron coating/low-activation steel;
2) Preparation of transition layer materials
Polishing and ultrasonically cleaning a transition layer material vanadium alloy foil belt, 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 coating with thickness of 5 μm,10 μm and 15 μm on the surface of low-activation steel by magnetron sputtering, and vacuum degree of 5×10 -3 Pa; vacuum packaging the vanadium foil strip and the low-activation steel sample after magnetron sputtering is completed;
3) Cleaning and assembling of parts to be welded
4) Polishing and ultrasonically cleaning a base metal tungsten alloy, air-drying, assembling a vanadium foil strip, a low-activation steel sample subjected to magnetron sputtering by adopting a tool, and the tungsten alloy into a sample from top to bottom according to the sequence of the tungsten alloy, the vanadium foil strip, the chromium coating and the low-activation steel, and placing the sample in a vacuum hot-pressing furnace;
4) Vacuum hot-pressing sintering
Heating rate of 10-20deg.C/min, and vacuum degree of less than 5×10 -3 Pa, sintering temperature is 700 ℃, and heat preservation time is as follows: the pressure was chosen to be 100MPa for 1h. Cooling to room temperature at a speed of less than 5 ℃ per minute after sintering to form a compact connecting joint; and (5) sintering the welding piece, and taking out the sample.
5) X-ray diffraction and microstructure analysis are carried out on the sintered sample interface, and the interface layer is generated in the series of samples according to the phase identification and the microstructure analysis result.
The invention can obtain the high-strength joint structure of the whole 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 distributed in a gradient way to the two sides of the low-activation steel and the tungsten alloy respectively, and the transition layer can form good bonding strength with the matrix. The invention can meet the requirement of researching the plasma-oriented component of the fusion reactor, and has important significance for the development of the component.
Claims (5)
1. A method for preparing a low-activation steel and tungsten complete solid solution joint, which is characterized by comprising the following steps:
step one: determination of transition layer material
Determining a transition layer material and a welding structure position according to the properties of a base material and the transition layer material;
step two: polishing and cleaning
Polishing and ultrasonic cleaning the transition layer material and the base material, and carrying out metal deposition on the surface of the base material;
step three: cleaning and assembly
Polishing and ultrasonically cleaning a base metal tungsten alloy, air-drying, assembling a vanadium alloy and a magnetron sputtered low-activation steel sample and a tungsten alloy from top to bottom in the sequence of tungsten alloy/vanadium alloy/chromium coating/low-activation steel by adopting a tool, and placing the samples in a vacuum hot-pressing furnace;
step four: vacuum hot-pressing sintering
Carrying out vacuum hot-pressing sintering on the product obtained in the step three;
the surface metal deposition of the base metal in the second step is performed by using a magnetron sputtering mode;
the magnetron sputtering mode is that the vacuum degree is 5 multiplied by 10 -3 Under Pa;
the magnetron sputtering is to deposit chromium coating on the surface of the base material;
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 welding structure is tungsten alloy/vanadium alloy/chromium coating/low-activation steel;
the vacuum hot-pressed sintering refers to sintering parameters as follows: the heating rate is 10-20deg.C/min, and the vacuum degree is less than 5×10 - 3 Pa, sintering temperature is 700-760 ℃, and heat preservation time is as follows: 0.5-2 h, and the pressure is 100Mpa.
2. A method of making a low activation steel and tungsten complete solid solution joint as defined in claim 1 wherein: and after sintering, cooling to room temperature at a speed of less than 5 ℃ per minute.
3. A method of making a low activation steel and tungsten complete solid solution joint as defined in claim 2 wherein: the purity of the vanadium alloy was 99.9%.
4. A method of making a low activation steel and tungsten complete solid solution joint as defined in claim 3 wherein: the thickness of the vanadium alloy is 1mm-2mm.
5. The method for preparing the low-activation steel and tungsten complete solid solution joint as claimed in claim 4, wherein the method comprises the following steps: the thickness of the chromium coating deposited on the low-activation steel by magnetron sputtering is 5-15 mu m.
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| CN115194146B (en) * | 2022-07-22 | 2023-11-17 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Functionally graded layer material suitable for fusion reactor tungsten and steel connection |
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| CN106825583A (en) * | 2016-12-30 | 2017-06-13 | 中南大学 | A kind of tungsten and low activation stainless steel nanometer gradient composite connecting method |
| CN108788436B (en) * | 2018-06-05 | 2021-02-09 | 中国科学院合肥物质科学研究院 | Process for diffusion bonding of fusion reactor material tungsten and steel by using hydrogen-containing metal |
| CN109396631B (en) * | 2018-11-14 | 2020-12-11 | 中国工程物理研究院材料研究所 | Hot isostatic pressing diffusion bonding method for tungsten/transition layer/stainless steel |
| CN111347146B (en) * | 2018-12-24 | 2022-05-20 | 核工业西南物理研究院 | Tungsten and heat sink material connector and preparation method thereof |
| CN111347147B (en) * | 2018-12-24 | 2022-05-20 | 核工业西南物理研究院 | Hot isostatic pressing connection method of tungsten and heat sink material |
| CN109604802A (en) * | 2019-01-03 | 2019-04-12 | 中国兵器工业第五九研究所 | The connection method of tungsten or tungsten alloy and steel, the connection method of profile and sectional material joint |
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