A method for preparing a plate type tungsten-copper module in a nuclear fusion divertor device

Abstract

The application discloses a preparation method of a flat plate type tungsten copper module in a nuclear fusion filter device, and the method comprises the following steps: firstly, taking tungsten sheets and cleaning; secondly, uniformly mixing Cu powder, Cr powder and Zr powder to obtain CuCrZr mixed powder; thirdly, sequentially placing the cleaned tungsten sheets, copper powder and CuCrZr mixed powder into a mold to carry out discharge plasma sintering to obtain a composite block; fourthly, carrying out heat treatment on the composite block; and fifthly, carrying out hot isostatic pressing treatment on the heat-treated composite block and a CuCrZr block to obtain the flat plate type tungsten copper module. The W / Cu / CuCrZr material is prepared by adopting the SPS sintering method, the W / Cu / CuCrZr-CuCrZr tungsten copper module is obtained by combining the hot isostatic pressing method with the CuCrZr block, the introduction of intermediate phases and impurities such as Ni is reduced, the heat conduction capacity of the tungsten copper module is ensured, the bonding strength of the tungsten copper module is improved, the tungsten copper module is suitable for use in the nuclear fusion filter device, and the method has few processes and low cost.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of material preparation, and particularly relates to a preparation method of a flat plate type tungsten-copper module in a nuclear fusion divertor device. BACKGROUND

[0002] Energy is the cornerstone of national economic development, and with the continuous progress of social development, the demand for energy is gradually increasing. However, the available amount of traditional energy fuels is decreasing year by year, so developing new energy has become an important task. Many countries around the world jointly participated in the construction of the world's largest international thermonuclear experimental reactor (ITER) program. The plasma-facing component (PFC) is an important component in ITER, and its surface heat flux is as high as 20 MW / m 2 in its working environment. The existing single material cannot normally serve in this environment, so it is necessary to connect different performance materials in a layered composite. The PFC is mainly composed of a plasma-facing material (PFM) and a heat sink material (HSM). Tungsten has high melting point, low vapor pressure, low sputtering rate and low tritium retention, so it is used as a plasma-facing material. Cu has high thermal conductivity, high electrical conductivity and other advantages, so it is used as a heat sink material. The tungsten-copper module is currently recognized as the most promising type of plasma-facing component for nuclear fusion reactors.

[0003] The traditional preparation method of the tungsten-copper module is to first prepare an oxygen-free copper layer on the surface of the tungsten sheet, and then composite the oxygen-free copper layer with CuCrZr to obtain a flat plate type tungsten-copper module. The common method for preparing an oxygen-free copper layer on the surface of the tungsten sheet is vacuum casting and brazing. Although the vacuum casting process is simple, it requires complex machining treatment in the later stage, and in addition, the oxygen-free copper surface after casting is prone to shrinkage and other defects, and also needs to be subjected to hot isostatic pressing or hot pressing to reshape the surface shrinkage. Brazing introduces other impurities, reducing the heat transfer capacity of the PFC and affecting its service life. The common connection method for the oxygen-free copper layer and the CuCrZr is brazing or hot isostatic pressing. Brazing introduces impurity elements, reducing the thermal conductivity; hot isostatic pressing also requires preparing a Ni layer on the surface of the oxygen-free copper in advance, which also affects the thermal conductivity of the PFC. SUMMARY

[0004] The technical problem to be solved by the present application is to provide a preparation method of a flat plate type tungsten-copper module in a nuclear fusion divertor device to solve the problems of the prior art. The method uses the SPS sintering method to prepare W / Cu / CuCrZr material, and combines the hot isostatic pressing method to connect it with the CuCrZr block to obtain a flat plate type tungsten-copper module of W / Cu / CuCrZr-CuCrZr, which reduces the introduction of intermediate phases and Ni impurities, improves the bonding strength of the flat plate type tungsten-copper module, ensures its thermal conductivity, and solves the problems of long process and easy introduction of impurities affecting the thermal conductivity of the tungsten-copper module in the prior art.

[0005] To solve the above technical problems, the technical scheme adopted by the present application is as follows: a preparation method of a flat plate type tungsten copper module in a nuclear fusion filter device, characterized in that the method comprises the following steps:

[0006] Step one, take tungsten sheet and clean the surface of the tungsten sheet;

[0007] Step two, mix Cu powder, Cr powder and Zr powder uniformly using a ball mill to obtain CuCrZr mixed powder;

[0008] Step three, sequentially place the cleaned tungsten sheet in step one, copper powder and CuCrZr mixed powder obtained in step two into a mold for discharge plasma sintering to obtain a composite block body with a CuCrZr layer;

[0009] Step four, heat treat the composite block body obtained in step three;

[0010] Step five, place the CuCrZr layer in the heat treated composite block body in step four opposite to the CuCrZr block body and put them into a package, and then perform hot isostatic pressing treatment to obtain a flat plate type tungsten copper module in a nuclear fusion filter device.

[0011] The preparation method of the flat plate type tungsten copper module in the nuclear fusion filter device described above is characterized in that the tungsten sheet in step one has a processed structure with grain orientation perpendicular to the rolling direction. The tungsten sheet with this structure has fewer grain boundaries and good thermal conductivity.

[0012] The preparation method of the flat plate type tungsten copper module in the nuclear fusion filter device described above is characterized in that the cleaning in step one is ultrasonic cleaning. Generally, ultrasonic cleaning is performed until there is no foreign matter or oxidation on the surface of the tungsten sheet.

[0013] The preparation method of the flat plate type tungsten copper module in the nuclear fusion filter device described above is characterized in that the Cr powder addition amount in the CuCrZr mixed powder in step two is 0.6% to 1%, and the Zr powder addition amount is 0.08% to 0.12%. The block body prepared from the CuCrZr mixed powder with this composition meets the ITER performance requirements.

[0014] The preparation method of the flat plate type tungsten copper module in the nuclear fusion filter device described above is characterized in that the discharge plasma sintering temperature in step three is 750°C to 850°C, the pressure is 30MPa to 50MPa, and the sintering time is 20min to 30min. The copper alloy composite block body prepared under this discharge plasma sintering process parameter has high density and good performance, especially high thermal conductivity.

[0015] The preparation method of the plate type tungsten copper module in the nuclear fusion filter device has the characteristics that the heat treatment in the step four includes vacuum solid solution treatment and aging treatment in argon atmosphere, the temperature of the vacuum solid solution treatment is 880-920 DEG C, the time is 0.5-1h, the temperature of the aging treatment in argon atmosphere is 400-500 DEG C, and the time is 4-5h.

[0016] The preparation method of the plate type tungsten copper module in the nuclear fusion filter device has the characteristics that the heat treatment in the step four includes vacuum solid solution treatment and aging treatment in argon atmosphere, the temperature of the vacuum solid solution treatment is 880-920 DEG C, the time is 0.5-1h, the temperature of the aging treatment in argon atmosphere is 400-500 DEG C, and the time is 4-5h.

[0017] Compared with the prior art, the present application has the following advantages:

[0018] 1、The present application first uses the spark plasma sintering (SPS) method to prepare the composite block, i.e., the W / Cu / CuCrZr material, and then uses the hot isostatic pressing method to connect the composite block with the CuCrZr block to obtain the plate type tungsten copper module. The conventional W-Cu-Ni-CuCrZr connection is changed into the W / Cu / CuCrZr-CuCrZr connection, the introduction of the intermediate phase and impurities such as Ni is reduced, the heat conduction capacity of the product plate type tungsten copper module is ensured, and the high bonding strength of the product plate type tungsten copper module is ensured through the solid phase diffusion between the CuCrZrs, so that the plate type tungsten copper module is suitable for use in the nuclear fusion filter device.

[0019] 2、The present application uses the SPS sintering method to prepare the composite block, i.e., the W / Cu / CuCrZr material. The tail end of the composite block does not have defects such as shrinkage holes, the process of treating the shrinkage holes is reduced, the production efficiency is improved, and the production cost is reduced.

[0020] 3、The present application performs heat treatment on the W / Cu / CuCrZr material to effectively remove the processing stress and restore the performance, so that the plate type tungsten copper module does not have defects such as cracks during the service process.

[0021] 4、The SPS sintering process and the hot isostatic pressing process of the present application are performed in a vacuum environment, so that other impurities are not introduced or oxidation does not occur, the strength of the bonding interface is greatly improved, the plate type tungsten copper module has high bonding strength and heat conduction capacity, and the plate type tungsten copper module has good thermal fatigue life performance.

[0022] 5、The present application has few processes, the raw materials are easy to obtain, and the cost is low, so that the preparation difficulty is reduced and the practicability of the method is improved.

[0023] The technical solutions of the present application are described in further detail below through examples. DETAILED DESCRIPTION

[0024] Example 1

[0025] The present example comprises the following steps:

[0026] Step one, take tungsten sheet and ultrasonic clean the surface of the tungsten sheet; the organization of the tungsten sheet is in a processed state, and the grain orientation is perpendicular to the rolling direction;

[0027] Step two, mix Cu powder, Cr powder and Zr powder with mass purity of 99.99% uniformly using a ball mill to obtain CuCrZr mixed powder; the addition amount of Cr powder in the CuCrZr mixed powder is 1%, the addition amount of Zr powder is 0.08%, and the addition amount of Cu powder is 98.92%;

[0028] Step three, first place the cleaned tungsten sheet in step one at the bottom of the mold, then spread copper powder with mass purity of 99.99% on the tungsten sheet, then spread the CuCrZr mixed powder obtained in step two on the copper powder, and pad a layer of graphite sheet at the place where the upper and lower pressing heads of the mold contact the powder, and then put it into a discharge plasma equipment for discharge plasma sintering to obtain a composite block body, i.e. W / Cu / CuCrZr material; the temperature of the discharge plasma sintering is 750℃, the pressure is 50MPa, and the sintering time is 20min;

[0029] Step four, first perform vacuum solid solution treatment on the composite block body obtained in step three, and then perform aging treatment in an argon atmosphere; the temperature of the vacuum solid solution treatment is 880℃, and the time is 1h; the temperature of the aging treatment in the argon atmosphere is 400℃, and the time is 5h;

[0030] Step five, place the CuCrZr layer of the composite block body after heat treatment in step four opposite to the CuCrZr block body and put it into a can, and then perform hot isostatic pressing treatment to obtain a flat plate type tungsten copper module in a nuclear fusion divertor device; the temperature of the hot isostatic pressing treatment is 600℃, the time is 2h, and the pressure is 150MPa.

[0031] Example 2

[0032] The present example comprises the following steps:

[0033] Step one, take tungsten sheet and ultrasonic clean the surface of the tungsten sheet; the organization of the tungsten sheet is in a processed state, and the grain orientation is perpendicular to the rolling direction;

[0034] Step two, use a ball mill to mix Cu powder, Cr powder and Zr powder with mass purity of 99.99% to obtain CuCrZr mixed powder; the adding amount of Cr powder in the CuCrZr mixed powder is 0.8%, the adding amount of Zr powder is 0.1%, and the adding amount of Cu powder is 99.1%;

[0035] Step three, first, place the cleaned tungsten sheet in step one at the bottom of the mold, then spread copper powder with mass purity of 99.99% on the tungsten sheet, then spread the CuCrZr mixed powder obtained in step two on the copper powder, and pad a layer of graphite sheet at the place where the upper and lower press heads of the mold contact the powder, and then put it into the discharge plasma equipment for discharge plasma sintering to obtain a composite block body, i.e. W / Cu / CuCrZr material; the temperature of the discharge plasma sintering is 800℃, the pressure is 40MPa, and the sintering time is 25min;

[0036] Step four, first, perform vacuum solid solution treatment on the composite block body obtained in step three, and then perform aging treatment in an argon atmosphere; the temperature of the vacuum solid solution treatment is 900℃, and the time is 0.75h; the temperature of the aging treatment in the argon atmosphere is 450℃, and the time is 4.5h;

[0037] Step five, place the CuCrZr layer opposite to the CuCrZr block in the composite block body after heat treatment in step four into a package, and then perform hot isostatic pressing treatment to obtain a flat plate type tungsten copper module in the nuclear fusion divertor device; the temperature of the hot isostatic pressing treatment is 650℃, the time is 2.5h, and the pressure is 125MPa.

[0038] Example 3

[0039] This example includes the following steps:

[0040] Step one, take a tungsten sheet and ultrasonically clean the surface of the tungsten sheet; the organization of the tungsten sheet is in a processed state, and the grain orientation is perpendicular to the rolling direction;

[0041] Step two, use a ball mill to mix Cu powder, Cr powder and Zr powder with mass purity of 99.99% to obtain CuCrZr mixed powder; the adding amount of Cr powder in the CuCrZr mixed powder is 0.6%, the adding amount of Zr powder is 0.12%, and the adding amount of Cu powder is 99.28%;

[0042] Step three, first, the cleaned tungsten sheet in step one is placed at the bottom of the mold, then the copper powder with mass purity of 99.99% is laid on the tungsten sheet, then the CuCrZr mixed powder obtained in step two is laid on the copper powder, and a layer of graphite sheet is laid on the contact place between the upper and lower press heads of the mold and the powder, then the discharge plasma equipment is put into the discharge plasma sintering to obtain the composite block, i.e. the W / Cu / CuCrZr material; the temperature of the discharge plasma sintering is 850℃, the pressure is 30MPa, and the sintering time is 30min;

[0043] Step four, the composite block obtained in step three is first subjected to vacuum solid solution treatment, and then subjected to aging treatment under argon atmosphere; the temperature of the vacuum solid solution treatment is 920℃, and the time is 0.5h; the temperature of the aging treatment under argon atmosphere is 500℃, and the time is 4h;

[0044] Step five, the CuCrZr layer of the composite block after heat treatment in step four is opposite to the CuCrZr block, and the composite block is loaded into a package, then hot isostatic pressing treatment is carried out to obtain the plate type tungsten copper module in the nuclear fusion divertor device; the temperature of the hot isostatic pressing treatment is 700℃, the time is 3h, and the pressure is 100MPa.

[0045] The above is only the preferred embodiment of the present application, and does not limit the present application. Any simple modification, change and equivalent change according to the technical essence of the present application to the above embodiment are still within the protection scope of the technical solution of the present application.

Claims

1. A method for producing a plate-type tungsten-copper module in a nuclear fusion divertor apparatus, characterized by, The method comprises the following steps: Step one, take tungsten sheet and clean the surface of the tungsten sheet; Step two, use a ball mill to mix Cu powder, Cr powder and Zr powder uniformly to obtain CuCrZr mixed powder; the addition amount of Cr powder in the CuCrZr mixed powder is 0.6%~1%, and the addition amount of Zr powder is 0.08%~0.12%; Step three, put the cleaned tungsten sheet in step one, copper powder and CuCrZr mixed powder obtained in step two into a mold in sequence for discharge plasma sintering to obtain a composite block body with a CuCrZr layer; the temperature of the discharge plasma sintering is 750℃~850℃, the pressure is 30MPa~50MPa, and the sintering time is 20min~30min; Step four, heat treat the composite block body obtained in step three; Step five, place the CuCrZr layer and the CuCrZr block body in the composite block body after heat treatment in step four opposite to each other and put them into a package, and then perform hot isostatic pressing treatment to obtain a flat plate type tungsten copper module in a nuclear fusion divertor device.

2. The method of claim 1, wherein the method is used for the preparation of a tungsten-copper plate module for a nuclear fusion divertor device, characterized in that, The tungsten sheet in step one has a processed structure, and the grain orientation is perpendicular to the rolling direction.

3. The method for preparing a planar tungsten-copper module in a nuclear fusion divertor device according to claim 1, characterized in that, The cleaning in step one is ultrasonic cleaning.

4. The method of claim 1, wherein the method is characterized by: The heat treatment in step four comprises vacuum solid solution treatment and aging treatment in an argon atmosphere; the temperature of the vacuum solid solution treatment is 880℃~920℃, and the time is 0.5h~1h; the temperature of the aging treatment in the argon atmosphere is 400℃~500℃, and the time is 4h~5h.

5. The method of claim 1, wherein the method is characterized by: The temperature of the hot isostatic pressing treatment in step five is 600℃~700℃, the time is 2h~3h, and the pressure is 100MPa~150MPa.