Device and method for plating nickel on surface of radioactive substrate at low temperature

Abstract

The invention provides a radioactive matrix surface low-temperature nickel plating device and method.The radioactive matrix surface low-temperature nickel plating device comprises a cleaning box assembly, the cleaning box assembly comprises a cleaning box body, a cleaning sample table, an ion source and a cleaning vacuumizing pipeline, an ion cleaning cavity is formed in the cleaning box body, and the cleaning sample table is arranged in the cleaning box body; a gate plate is arranged between the coating box assembly and the cleaning box assembly, the coating box assembly comprises a first box body and a first air inlet pipeline, and a first coating cavity is formed in the first box body; through the arrangement of the cleaning box assembly, ion cleaning of the whole surface of a workpiece can be achieved, natural oxide on the surface is removed, a metal substrate is exposed, the coating quality is improved, through the arrangement of the coating box assembly, the retention time of gas in the first coating cavity is prolonged, and the coating quality is improved. And coating deposition of a workpiece can be completed through sufficient reaction at a lower temperature, and the binding force of a coating film can be improved.

Description

Technical Field

[0001] The present application belongs to the field of nuclear industry technology, and specifically relates to a device and method for low-temperature nickel plating on the surface of a radioactive substrate. Background Art

[0002] There are some metals with relatively active chemical properties in radioactive materials. When in use, they are in contact with air for a long time, which is prone to oxidation corrosion, leading to material failure, radioactive aerosol escape, environmental pollution and excessive radiation dose to personnel. In order to ensure the safe use of radioactive materials, it is necessary to greatly improve the corrosion resistance. Usually, a layer of nickel metal coating is prepared on the surface of the radioactive metal substrate. The methods used include electroplating and chemical vapor deposition (CVD).

[0003] Electroplating is a method for preparing coatings in an aqueous solution environment. The device is relatively simple and can grow thicker films. However, due to the presence of water, it will react with the radioactive matrix material to release gas. The obtained coating is relatively loose and has a high porosity. At the same time, a large amount of radioactive waste liquid is produced. It is usually not used as a film that directly contacts the substrate. CVD is a vacuum coating method that can directly form a relatively dense nickel metal film on the surface of a radioactive substrate. However, when this process is used for coating the entire surface of a hemispherical workpiece, the gas continuously passes into the cavity, generating a constant flow field in the space. Affected by this, the film thickness of the workpiece is not uniform, especially in the area far away from the air inlet or on the back of the air inlet. There is a strong shadow effect and the film thickness is thin. At the same time, the coating temperature of CVD is relatively high, usually 250-400℃, which makes the thermal stress of the prepared film larger, and it is easy to bubble and crack during long-term use, resulting in failure of the substrate in direct contact with the corrosive medium. In addition, the substrate surface is not pretreated before coating, and the naturally existing oxides will also have a great impact on the coating quality. Summary of the invention

[0004] The present invention aims to solve at least one of the technical problems existing in the prior art or related art.

[0005] In order to solve the above problems, the first aspect of the present application provides a device for low-temperature nickel plating on the surface of a radioactive substrate, comprising:

[0006] A cleaning box assembly, the cleaning box assembly includes a cleaning box body, a cleaning sample stage, an ion source and a cleaning vacuum pipeline, the cleaning box body is provided with an ion cleaning chamber, the cleaning sample stage is arranged in the cleaning box body for placing workpieces, the ion source is arranged on the top and side walls of the cleaning box body, and its output end is located in the ion cleaning chamber, and the cleaning vacuum pipeline is connected to the cleaning box body;

[0007] A coating box assembly, wherein a gate plate is arranged between the coating box assembly and the cleaning box assembly, wherein the coating box assembly comprises a first box body and a first air inlet pipe, wherein a first coating cavity is opened inside the first box body, wherein a water cooling layer is arranged inside the first box body, wherein the first coating cavity is used for storing workpieces after being cleaned by the cleaning box assembly, and wherein the first air inlet pipe is connected to the first box body for supplying coating gas into the first box body.

[0008] Optionally, the coating box assembly further includes a first sample stage, which is disposed in the first coating chamber and is used for placing a workpiece.

[0009] Optionally, the first sample stage comprises:

[0010] A first supporting platform, wherein the first supporting platform is disposed in the first coating chamber;

[0011] a first telescopic support, the first telescopic support being symmetrically arranged on the first supporting platform;

[0012] The second telescopic support is symmetrically arranged on the first support platform and located outside the first telescopic support. The length of the second telescopic support is greater than that of the first telescopic support.

[0013] Optionally, the coating box assembly also includes a first heating element, which includes an induction heating source and an induction coil. The induction heating source is arranged on the top of the first box body, and the induction coil is connected to the induction heating source for heating the workpiece.

[0014] Optionally, the coating box assembly further includes a first vacuum pumping pipeline, the first vacuum pumping pipeline is connected to the coating box assembly, and the first vacuum pumping pipeline includes:

[0015] A first main pipeline, the first main pipeline is connected to the coating box assembly, and a first valve, a first vacuum gauge, a second valve, a first molecular pump, a third valve and a first mechanical pump are sequentially arranged on the first main pipeline;

[0016] A first branch pipeline, wherein the first end of the first branch pipeline is connected to the first main pipeline and is located between the second valve and the first molecular pump, the second end of the first branch pipeline is connected to the first main pipeline and is located between the third valve and the first mechanical pump, and a fourth valve is arranged on the first branch pipeline.

[0017] Optionally, the coating box assembly includes:

[0018] A second box body, wherein a second coating cavity is provided in the second box body, and a heating layer is provided outside the second box body;

[0019] A second sample stage, the second sample stage is disposed in the second coating chamber and is used to place the workpiece after being cleaned by the cleaning box assembly;

[0020] A second heating element, the second heating element is symmetrically arranged in the second coating chamber and located on both sides of the second sample stage;

[0021] A plasma source, wherein the plasma source is disposed on the top of the second housing;

[0022] A second air inlet pipeline, the second air inlet pipeline is connected to the second box and is used to supply coating gas into the first box;

[0023] The second vacuum pumping pipeline is connected to the second box.

[0024] Optionally, the second sample stage comprises:

[0025] A second supporting platform, wherein the second supporting platform is disposed in the second coating chamber;

[0026] a third telescopic support, the third telescopic support being symmetrically arranged on the second support platform;

[0027] A fourth telescopic support column is symmetrically arranged on the second support platform and is located outside the third telescopic support column. The length of the fourth telescopic support column is greater than that of the third telescopic support column.

[0028] Optionally, the second vacuum pumping pipeline includes:

[0029] a second main pipe, the second main pipe being connected to the second box, and the second main pipe being provided with a fifth valve, a second vacuum gauge, a sixth valve, a second molecular pump, a seventh valve and a second mechanical pump in sequence;

[0030] A second branch pipeline, the first end of the second branch pipeline is connected to the second main pipeline and is located between the fifth valve and the second molecular pump, the second end of the second branch pipeline is connected to the second main pipeline and is located between the sixth valve and the second mechanical pump, and an eighth valve is arranged on the second branch pipeline.

[0031] Optionally, a transmission component is provided on the cleaning box.

[0032] The second aspect of the present application provides a method for low-temperature nickel plating on a radioactive substrate surface, using a device for low-temperature nickel plating on a radioactive substrate surface as in any technical solution of the first aspect, comprising the following steps:

[0033] S1, placing the workpiece on the cleaning sample table in the cleaning box assembly to clean the sample;

[0034] S2. Put the cleaned workpiece into the coating box assembly, and introduce coating gas into the coating box assembly to coat the workpiece.

[0035] Beneficial Effects

[0036] An apparatus and method for low-temperature nickel plating on the surface of a radioactive substrate provided in an embodiment of the present invention can achieve ion cleaning of the entire surface of the workpiece through the setting of a cleaning box assembly, remove natural oxides on the surface, expose the metal substrate, and improve the quality of the coating. Through the setting of the coating box assembly, the gas can stay in the first coating chamber for a longer time, so that the coating deposition of the workpiece can be fully reacted at a lower temperature, which is beneficial to improving the coating bonding strength. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 A structural diagram of an embodiment of the present application;

[0038] Figure 2 This is a structural diagram of a cleaning tank assembly in one embodiment of the present application;

[0039] Figure 3 This is a structural diagram of a coating box assembly in one embodiment of the present application;

[0040] Figure 4 This is a structural diagram of a coating box assembly according to another embodiment of the present application.

[0041] The reference numerals are:

[0042] 1. Cleaning box assembly; 2. Cleaning box body; 3. Cleaning sample stage; 4. Ion source; 5. Cleaning vacuum pipeline; 6. Coating box assembly; 7. Gate; 8. First box body; 9. First air inlet pipeline; 10. First sample stage; 11. First support platform; 12. First telescopic support pillar; 13. Second telescopic support pillar; 14. First heating element; 15. Induction heating source; 16. Induction coil; 17. First vacuum pipeline; 18. First main pipeline; 19. First valve; 20. First vacuum gauge; 21. Second valve; 22. First molecular pump; 23. Third valve; 24. The first mechanical pump; 25. The first branch pipeline; 26. The fourth valve; 27. The second box; 28. The second sample stage; 29. ​​The second heating element; 30. The plasma source; 31. The second air inlet pipeline; 32. The second vacuum pipeline; 33. The second support platform; 34. The third telescopic support; 35. The fourth telescopic support; 36. The second main pipeline; 37. The fifth valve; 38. The second vacuum gauge; 39. The sixth valve; 40. The second molecular pump; 41. The seventh valve; 42. The second mechanical pump; 43. The second branch pipeline; 44. The eighth valve; 45. The transmission element. DETAILED DESCRIPTION

[0043] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise" and the like, indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred system or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0044] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0045] In this application, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be the internal communication of two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0046] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0047] See also Figure 1-4 As shown, according to the first aspect of the present application, an apparatus for low-temperature nickel plating on a radioactive substrate surface is provided, comprising:

[0048] A cleaning box assembly 1, the cleaning box assembly 1 includes a cleaning box body 2, a cleaning sample stage 3, an ion source 4 and a cleaning vacuum pipeline 5, the cleaning box body 2 is provided with an ion cleaning chamber, the cleaning sample stage 3 is arranged in the cleaning box body 2 for placing a workpiece, the ion source 4 is arranged on the top and side wall of the cleaning box body 2, and its output end is located in the ion cleaning chamber, and the cleaning vacuum pipeline 5 is connected to the cleaning box body 2;

[0049] A coating box assembly 6, wherein a gate plate 7 is arranged between the coating box assembly 6 and the cleaning box assembly 1, wherein the coating box assembly 6 comprises a first box body 8 and a first air inlet pipe 9, wherein a first coating cavity is provided inside the first box body 8, wherein a water cooling layer is provided inside the first box body 8, wherein the first coating cavity is used for storing workpieces cleaned by the cleaning box assembly 1, and wherein the first air inlet pipe 9 is connected to the first box body 8 for supplying coating gas into the first box body 8.

[0050] The device for low-temperature nickel plating on the surface of a radioactive substrate provided in this embodiment includes a cleaning box 2 assembly and a coating box assembly 6, which are connected by a gate plate 7 and are placed in a negative pressure exhaust glove box as a whole to prevent radioactive substances from leaking into the operating environment of personnel. The cleaning box assembly 1 is used to perform ion cleaning on the workpiece to remove the natural oxide on the surface and expose the metal substrate; the coating box assembly 6 is used to coat the cleaned workpiece.

[0051] The cleaning box body 2 of the cleaning box assembly 1 is made of high-strength, radiation-resistant and well-sealed materials. The ion source 4 arranged on the top and side walls of the cleaning box body 2 is a high-performance Kaufman source. The two cooperate with each other to bombard the workpiece placed on the cleaning sample stage 3 with ions from different angles. The ion energy, beam density and other parameters of the ion source 4 can be accurately adjusted according to the material and degree of contamination of the workpiece. The cleaning sample stage 3 has high-precision rotation and lifting functions, which are realized by motor drive and transmission mechanism to ensure that all parts of the workpiece can be fully processed during the cleaning process. The cleaning vacuum pipeline 5 connects the cleaning box body 2 with the external vacuum pump system, which can pump the air pressure in the ion cleaning chamber to a high vacuum degree to meet the requirements of ion cleaning.

[0052] The first coating chamber is provided inside the first box body 8 of the coating box assembly 6, and a water-cooling layer is provided outside the first coating chamber. The water-cooling layer adopts a spiral cooling water pipe layout, which can effectively take away the heat generated during the coating process and maintain the temperature in the chamber stable. The first air inlet pipeline 9 connects the first box body 8 with the external carbonyl nickel precursor supply system, which is a carbonyl nickel storage tank. The first air inlet pipeline 9 is equipped with an atomic layer deposition (ALD) valve, which is a millisecond-level pulse valve that can achieve pulsed entry of carbonyl nickel gas for a few milliseconds to tens of seconds. During the coating process, through the precise control of the valve, the gas molecules can relax freely and evenly in the chamber to carry out thin film deposition. Due to the setting of the first box body 8, the gas can stay in the first coating chamber for a longer time, so that the coating deposition of the workpiece can be fully reacted at a lower temperature, which is beneficial to improve the coating bonding strength.

[0053] When in use, before coating, the storage temperature of the carbonyl nickel storage tank is adjusted to -15°C, and the surface of the hemispherical workpiece is polished with 200, 400, and 800-grit sandpaper in the glove box protected by inert gas. Each time the sandpaper with different meshes is changed for polishing, it is necessary to ensure that the previous polishing marks can be covered. After polishing, the sample surface is wiped with anhydrous ethanol to ensure that there is no dust residue on the surface of the workpiece. The workpiece is placed on the cleaning sample table 3, the door of the cleaning box 2 is closed, and the first coating chamber and the cleaning chamber are evacuated to 5×10 -4 Pa, a rear gas supply pipeline is installed on the cleaning box 2, and 15 sccm argon gas is introduced into the cleaning chamber through the gas supply pipeline, and the gas pressure is adjusted to 1×10 -2 Pa to 3×10 -2 Pa, turn on the horizontal and vertical ion sources 4, adjust the ion beam current and anode current, turn on the rotation of the ion cleaning sample stage 3, and start cleaning the surface of the workpiece. Ten minutes later, use the transmission member 45 to turn the workpiece over and clean the other side. After cleaning, it can be placed in the coating box assembly 6 for coating.

[0054] By opening the gate 7, the first coating chamber can be connected to the cleaning chamber, and then the workpiece is transferred to the first coating chamber using the transmission member 45. The gate 7 is closed and carbonyl nickel gas is introduced into the first coating chamber through the first air inlet pipe 9 to deposit and coat the workpiece.

[0055] The coating box assembly 6 further includes a first sample stage 10 , which is disposed in the first coating chamber and is used for placing a workpiece.

[0056] The first sample stage 10 comprises:

[0057] A first supporting platform 11, wherein the first supporting platform 11 is disposed in the first coating chamber;

[0058] A first telescopic support 12, wherein the first telescopic support 12 is symmetrically arranged on the first supporting platform 11;

[0059] The second telescopic support 13 is symmetrically arranged on the first support platform 11 and located outside the first telescopic support 12 . The length of the second telescopic support 13 is greater than that of the first telescopic support 12 .

[0060] In this technical solution, the first sample table 10 is used to place the workpiece, and is composed of a first support platform 11, a first telescopic support 12 and a second telescopic support 13. The first support platform 11 provides a stable installation base for the first telescopic support 12 and the second telescopic support 13, and ensures the stability of the workpiece during the coating process. The first telescopic support 12 and the second telescopic support 13 support the workpiece from different positions by symmetrical arrangement, and because the length of the second telescopic support 13 is greater than the length of the first telescopic support 12, the synergistic effect of the two can realize the switching of the fulcrum during the coating process, effectively avoiding the problem that some parts of the workpiece cannot be deposited with a thin film due to the traditional fixed fulcrum, thereby achieving the effect of coating the entire surface without dead angles. It can be understood that the optimal number of the first telescopic support 12 and the second telescopic support 13 is four, which can stably support the workpiece from four positions at the bottom, and more conveniently realize the switching of the support. Furthermore, the first telescopic support 12 and the second telescopic support 13 can be electric push rods.

[0061] During use, the workpiece is placed on the first sample table 10, and the first air inlet pipe 9 supplies carbonyl nickel gas into the first coating chamber. The first sample table 10 can support the workpiece. At the same time, during the coating process, the height of the first telescopic support 12 or the second telescopic support 13 is adjusted every 20 minutes to replace the fulcrum, and the support is repeated continuously to complete the thin film deposition.

[0062] The coating box assembly 6 also includes a first heating element 14, which includes an induction heating source 15 and an induction coil 16. The induction heating source 15 is disposed on the top of the first box body 8, and the induction coil 16 is connected to the induction heating source 15 for heating the workpiece.

[0063] In this technical solution, the coating box assembly 6 includes a first heating element 14, which includes an induction heating source 15 and an induction coil 16. The induction heating source 15 is installed on the top of the first box 8, and the induction coil 16 is installed in the first box 8. The induction coil 16 is connected to the induction heating source 15, and the workpiece placed in the coating box is efficiently and evenly heated by the principle of electromagnetic induction.

[0064] When in use, after placing the workpiece on the first sample table 10, before introducing carbonyl nickel gas through the first air inlet pipe 9, first turn on the induction heating power supply, gradually increase the temperature to 180°C at a heating rate of 5°C / min, and then keep warm at 180°C for 1 hour to improve the uniformity of temperature distribution of various parts of the workpiece, and then introduce carbonyl nickel gas through the first air inlet pipe 9 to achieve coating of the workpiece.

[0065] The coating box assembly 6 further includes a first vacuum pumping pipeline 17, which is connected to the coating box assembly 6. The first vacuum pumping pipeline 17 includes:

[0066] A first main pipeline 18, the first main pipeline 18 is connected to the coating box assembly 6, and a first valve 19, a first vacuum gauge 20, a second valve 21, a first molecular pump 22, a third valve 23 and a first mechanical pump 24 are sequentially arranged on the first main pipeline 18;

[0067] A first branch pipeline 25, a first end of the first branch pipeline 25 is connected to the first main pipeline 18 and is located between the second valve 21 and the first molecular pump 22, a second end of the first branch pipeline 25 is connected to the first main pipeline 18 and is located between the third valve 23 and the first mechanical pump 24, and a fourth valve 26 is provided on the first branch pipeline 25.

[0068] In this technical solution, before heating by the first heating element 14, the pulse valve on the first air inlet pipeline 9 is opened first, and the valve on the carbonyl nickel storage tank is in a closed state. The first air inlet pipeline 9 and the first coating chamber are evacuated for 1 to 10 minutes through the first vacuum pumping pipeline 17 until the reading of the first vacuum gauge 20 is stable, so as to prevent the residual air in the first air inlet pipeline 9 from contaminating the film. It is determined that the vacuum is less than 5×10 -4 Pa, and then the first coating chamber is heated by the first heating element 14. After being heated to 180°C and kept warm for 1h, carbonyl nickel gas is introduced through the first air inlet line 9. The ventilation time, pressure holding time and exhaust time are set to 5s / 30s / 30s. It can be understood that the valve on the first air inlet line 9 is opened for 5s, the valve on the first vacuum line 17 is closed, and carbonyl nickel gas is introduced into the first coating chamber at a flow rate of 100sccm. Then the first air inlet line 9 and the first vacuum line 17 are closed for 30s to allow the introduced carbonyl nickel gas to react completely. Then the first vacuum line 17 is opened for 30s to exhaust the residual gas in the first coating chamber, and the air pressure is pumped to 5×10 -4Pa, that is, the air pressure is restored to the air pressure without the introduction of carbonyl nickel gas. This is a ventilation cycle. Repeating this cycle can achieve controllable and uniform deposition of the thickness of the metal nickel film. The ventilation time, pressure holding time and exhaust time in the cycle can be adjusted according to the type of deposited film and the size of the cavity to achieve the corresponding purpose. At the same time, if the first molecular pump 22 used in the first vacuum pipeline 17 cannot withstand the impact of a high content of nickel metal particles, the first molecular pump 22 can also be turned off during the coating process, and only the first mechanical pump 24 is used for vacuuming. At this time, the stable air pressure after one cycle is the limit air pressure drawn by the first mechanical pump 24.

[0069] The coating box assembly 6 includes:

[0070] A second box 27, wherein a second coating cavity is provided in the second box 27, and a heating layer is provided outside the second box 27;

[0071] A second sample stage 28, which is disposed in the second coating chamber and is used to place the workpiece after being cleaned by the cleaning box assembly 1;

[0072] A second heating element 29, which is symmetrically disposed in the second coating chamber and located on both sides of the second sample stage 28;

[0073] A plasma source 30, wherein the plasma source 30 is disposed on the top of the second box 27;

[0074] A second air inlet pipeline 31, which is connected to the second box 27 and is used to feed the coating gas into the first box 8;

[0075] The second vacuum line 32 is connected to the second box 27 .

[0076] In this technical solution, the structure of the coating box assembly 6 can also include a second box body 27, a second sample table 28, a second heating element 29, a plasma source 30, a second air inlet pipe 31 and a second vacuum pipe 32. A second coating cavity is opened inside the second box body 27 to provide space for workpiece coating, and a heating layer arranged on the outside thereof helps to maintain a suitable temperature environment in the coating cavity.

[0077] The second sample stage 28 is placed in the second coating chamber, providing a stable placement for the cleaned workpiece. The second heating elements 29 symmetrically arranged in the second coating chamber and located on both sides of the second sample stage 28 can evenly heat the workpiece from both sides, further ensuring the temperature condition of the workpiece during the coating process. It can be understood that the second heating element 29 is a resistance heating plate, and the second heating element 29 is vertically installed on both sides of the second sample stage 28, which can heat the workpiece from both sides, making it more convenient and stable to adjust the heating temperature.

[0078] The plasma source 30 is located at the top of the second box 27 to provide the required plasma environment for coating. The second air inlet line 31 is connected to the second box 27 to accurately introduce the coating gas into the first box 8 to ensure the smooth coating reaction. In addition, the plasma source 30 can be used for enhanced chemical gas deposition and can reduce the required coating temperature in the second box 27. The second vacuum line 32 is connected to the second box 27 to maintain the pressure environment in the second coating chamber as needed during use.

[0079] The second sample stage 28 comprises:

[0080] A second supporting platform 33, wherein the second supporting platform 33 is disposed in the second coating chamber;

[0081] A third telescopic support 34, wherein the third telescopic support 34 is symmetrically arranged on the second support platform 33;

[0082] The fourth telescopic support 35 is symmetrically arranged on the second support platform 33 and is located outside the third telescopic support 34 . The length of the fourth telescopic support 35 is greater than that of the third telescopic support 34 .

[0083] In this technical solution, the second sample table 28 is used to place the workpiece, and is composed of a second support platform 33, a third telescopic support 34 and a fourth telescopic support 35. The second support platform 33 provides a stable installation base for the third telescopic support 34 and the fourth telescopic support 35, and ensures the stability of the workpiece placement during the coating process. The third telescopic support 34 and the fourth telescopic support 35 support the workpiece from different positions by symmetrical arrangement, and because the length of the fourth telescopic support 35 is greater than that of the third telescopic support 34, the synergistic effect of the two can realize the switching of the fulcrum during the coating process, effectively avoiding the problem that some parts of the workpiece cannot be deposited with a thin film due to the traditional fixed fulcrum, thereby achieving the effect of coating the entire surface without dead angles. It can be understood that the optimal number of the third telescopic support 34 and the fourth telescopic support 35 is four, which can stably support the workpiece from four positions at the bottom, and more conveniently realize the switching of the support.

[0084] Furthermore, the third telescopic support 34 and the fourth telescopic support 35 may be electric push rods.

[0085] The second vacuum pumping line 32 includes:

[0086] A second main pipe 36, the second main pipe 36 is connected to the second box 27, and a fifth valve 37, a second vacuum gauge 38, a sixth valve 39, a second molecular pump 40, a seventh valve 41 and a second mechanical pump 42 are sequentially arranged on the second main pipe 36;

[0087] A second branch pipeline 43, a first end of the second branch pipeline 43 is connected to the second main pipeline 36 and is located between the fifth valve 37 and the second molecular pump 40, a second end of the second branch pipeline 43 is connected to the second main pipeline 36 and is located between the sixth valve 39 and the second mechanical pump 42, and an eighth valve 44 is provided on the second branch pipeline 43.

[0088] In this technical solution, the second vacuum pumping line 32 is used to exhaust the second coating chamber according to usage requirements. Through the arrangement of the second main line 36 and the second branch line 43, if the second molecular pump 40 on the second main line 36 cannot withstand the impact of a high content of nickel metal particles, the second molecular pump 40 can also be closed during the coating process, and only the second mechanical pump 42 can be used for vacuuming, which is more flexible and convenient to use.

[0089] The cleaning box 2 is provided with a transmission member 45 .

[0090] In this technical solution, the transmission member 45 includes a handle and a U-shaped fork connected to the handle. The staff takes the transmission member 45 through the handle and transfers the workpiece from the cleaning chamber to the coating box assembly 6 through the fork.

[0091] The gas extracted by cleaning the vacuum pumping pipeline 5, the first vacuum pumping pipeline 17 and the second vacuum pumping pipeline 32 will be fed into the tail gas treatment device to avoid being directly discharged into the atmosphere to cause environmental pollution.

[0092] A second aspect of the present application provides a method for low-temperature nickel plating on a radioactive substrate surface, using the device for low-temperature nickel plating on a radioactive substrate surface in any embodiment of the first aspect, comprising the following steps:

[0093] S1, placing the workpiece on the cleaning sample table 3 in the cleaning box assembly 1, and cleaning the sample;

[0094] In this technical solution, before coating, the storage temperature of the carbonyl nickel storage tank is adjusted to -15°C, the negative pressure in the glove box is adjusted to -300 to -500 Pa, the inside of the cleaning box assembly 1 and the inside of the coating box assembly 6 are cleaned with anhydrous ethanol, and heated to 200°C for 5 hours after cleaning to remove adsorbed impurities and water vapor. In the glove box protected by inert gas, the surface of the hemispherical workpiece is polished with 200, 400, and 800 mesh sandpapers in turn. Each time the sandpaper with different meshes is changed for polishing, it is necessary to ensure that the previous polishing marks can be covered. After polishing, the sample surface is wiped with anhydrous ethanol to ensure that there is no dust residue on the sample surface. The workpiece is placed on the cleaning sample table 3, and the door of the cleaning box 2 is closed;

[0095] Open the cleaning vacuum line 5 and the first vacuum line 17 to vacuum the cleaning chamber and the first coating chamber, and gradually pump the air pressure to 5×10 -4 Below Pa;

[0096] 15 sccm of argon gas was introduced into the cleaning box through the gas supply pipe on the cleaning box 2, and the gas pressure was adjusted to 1×10 -2 Pa to 3×10 -2 Pa, turn on the horizontally and vertically placed ion sources 4, adjust the ion beam current and anode current, start the rotation of the cleaning sample stage 3, and start cleaning the surface of the workpiece. After ten minutes, use the sample transmission part 45 to turn the sample over and clean the other side. After cleaning, stop the rotation of the cleaning sample stage 3, open the gate 7, use the transmission part 45 to transfer the workpiece to the coating box assembly 6, and then the transmission part 45 retracts into the cleaning box 2 and closes the gate 7.

[0097] S2. Put the cleaned workpiece into the coating box assembly 6, and introduce coating gas into the coating box assembly 6 to coat the workpiece.

[0098] In this technical solution, when the workpiece is transferred to the coating box assembly 6 using the transmission member 45, it is necessary to ensure that the position of the induction coil 16 does not hinder the movement of the transmission rod. The induction heating source 15 is equipped with a controller, which can adjust the position of the induction coil 16 according to the use requirements, so that the workpiece is conveniently placed on the first support table 11. After the workpiece is transferred, the gate 7 is closed, and the pulse valve on the first air inlet line 9 is opened. The first air inlet line 9 connecting the carbonyl nickel storage tank and the coating cavity is evacuated for 1 to 10 minutes until the vacuum gauge reading is stable, so as to prevent the residual air in the first air inlet line 9 from contaminating the coating. Furthermore, at this time, the valve on the carbonyl nickel storage tank is in a closed state, so the first coating cavity can be evacuated. After determining that the vacuum in the first coating cavity is lower than 5×10 -4Pa, turn on the first heating element 14 to heat the first coating chamber, gradually raise the temperature to 180°C at a heating rate of 5°C / min, and then keep it at 180°C for 1h to improve the uniformity of temperature distribution of various parts of the workpiece;

[0099] The air flow rate of the first air inlet line 9 is set to 100 sccm, and the ventilation time, pressure holding time and exhaust time are set to 5s / 30s / 30s. It can be understood that the valve of the first air inlet line 9 is opened for 5s, the valve of the first vacuum line 17 is closed, and a certain amount of carbonyl nickel gas is introduced into the coating chamber at a flow rate of 100 sccm, and then the valves on the first air inlet line 9 and the valves on the first vacuum line 17 are closed for 30s to allow the introduced carbonyl nickel gas to react completely, and then the valve on the first vacuum line 17 is opened for 30s to exhaust the residual gas in the first coating chamber, and the air pressure is pumped to 5×10 -4 Pa, that is, the air pressure is restored to the pressure before the introduction of carbonyl nickel gas. This is a ventilation cycle. Repeating this cycle can achieve controllable and uniform deposition of the thickness of the metal nickel film. The ventilation time, pressure holding time and exhaust time in the cycle can be adjusted according to the type of deposited film and the size of the cavity to achieve the corresponding purpose. At the same time, if the first molecular pump 22 used cannot withstand the impact of a high content of nickel metal particles, the first molecular pump 22 can also be turned off during the coating process, and only the first mechanical pump 24 can be used for vacuum extraction. At this time, the stable air pressure after one cycle is the limit air pressure drawn by the first mechanical pump 24. If a carrier gas is used in the coating process, the stable air pressure after one cycle is the equilibrium air pressure after the carrier gas is introduced;

[0100] During the coating process of the workpiece, the first telescopic support 12 or the second telescopic support 13 on the first sample stage 10 is adjusted every 20 minutes to complete the replacement of the fulcrum of the workpiece to avoid the failure of film deposition at the fulcrum;

[0101] After the coating is completed, the heating of the first heating element 14 is stopped, and 30 sccm of Ar is continuously introduced into the first coating chamber to increase the cooling rate of the workpiece. After the workpiece is cooled to room temperature, Ar is introduced into the first coating chamber to atmospheric pressure, the workpiece is taken out of the furnace, and the entire coating process is completed.

[0102] In this embodiment, the coating box assembly 6 can also be a second box 27, a second sample table 28, a second heating element 29, a plasma source 30, a second air inlet pipeline 31 and a second vacuum pipeline 32, and the coating method is:

[0103] Before coating, the storage temperature of the carbonyl nickel storage tank is adjusted to -15°C, and the negative pressure in the glove box is adjusted to -300 to -500 Pa. The inside of the cleaning box component 1 and the coating box component 6 are cleaned with anhydrous ethanol. After cleaning, they are heated to 200°C and kept warm for 5 hours to remove adsorbed impurities and water vapor. In the glove box protected by inert gas, the surface of the hemispherical workpiece is polished with 200, 400, and 800 mesh sandpapers in turn. Each time the sandpaper with different meshes is changed for polishing, it is necessary to ensure that the previous polishing marks can be covered. After polishing, the sample surface is wiped with anhydrous ethanol to ensure that there is no dust residue on the sample surface. The workpiece is placed on the cleaning sample table 3 and the door of the cleaning box 2 is closed;

[0104] Open the cleaning vacuum line 5 and the second vacuum line 32 to vacuum the cleaning chamber and the second coating chamber, and gradually pump the air pressure to 5×10 -4 Below Pa;

[0105] 15 sccm of argon gas was introduced into the cleaning box through the gas supply pipe on the cleaning box 2, and the gas pressure was adjusted to 1×10 -2 Pa to 3×10 -2 Pa, turn on the horizontally and vertically placed ion sources 4, adjust the ion beam current and the anode current, turn on the rotation of the cleaning sample stage 3, and start cleaning the surface of the workpiece. After ten minutes, use the sample transmission member 45 to turn the sample over and clean the other side. After the cleaning is completed, stop the rotation of the cleaning sample stage 3, open the gate 7, use the transmission member 45 to transfer the workpiece to the coating box assembly 6, and then the transmission member 45 returns to the cleaning box 2 and closes the gate 7;

[0106] When the workpiece is transferred to the coating box assembly 6 using the transmission member 45, the workpiece is placed on the second sample table 28. After the workpiece is transferred, the gate 7 is closed, the pulse valve on the second air inlet line 31 is opened, and the second air inlet line 31 connecting the carbonyl nickel storage tank and the coating chamber is evacuated for 1 to 10 minutes until the vacuum gauge reading is stable, so as to prevent the residual air in the second air inlet line 31 from contaminating the coating. Furthermore, at this time, the valve on the carbonyl nickel storage tank is in a closed state, so the second coating chamber can be evacuated. After determining that the vacuum in the second coating chamber is less than 5×10 -4 Pa, turn on the second heating element 29 to heat the second coating chamber, gradually raise the temperature to 180°C at a heating rate of 5°C / min, and then keep it at 180°C for 1h to improve the uniformity of temperature distribution of each part of the workpiece. The second heating element 29 on the second heating element is vertically installed on both sides of the second sample stage 28, which can heat the workpiece from both sides, making it more convenient and stable to adjust the heating temperature. Moreover, through the setting of the plasma source 30, it can be used for enhanced chemical gas sample deposition, which can reduce the required coating temperature in the second box 27;

[0107] The air flow rate of the second air inlet line 31 is set to 100 sccm, and the ventilation time, pressure holding time and exhaust time are set to 5s / 30s / 30s. It can be understood that the valve of the second air inlet line 31 is opened for 5s, the valve of the second vacuum line 32 is closed, and a certain amount of carbonyl nickel gas is introduced into the coating chamber at a flow rate of 100 sccm, and then the valves on the second air inlet line 31 and the valves on the second vacuum line 32 are closed for 30s to allow the introduced carbonyl nickel gas to react completely, and then the valve on the second vacuum line 31 is opened for 30s to exhaust the residual gas in the second coating chamber, and the air pressure is pumped to 5×10 -4 Pa, that is, the air pressure is restored to the pressure before the introduction of carbonyl nickel gas. This is a ventilation cycle. Repeating this cycle can achieve controllable and uniform deposition of the thickness of the metal nickel film. The ventilation time, pressure holding time and exhaust time in the cycle can be adjusted according to the type of deposited film and the size of the cavity to achieve the corresponding purpose. At the same time, if the second molecular pump 40 used cannot withstand the impact of a high content of nickel metal particles, the second molecular pump 40 can also be turned off during the coating process, and only the second mechanical pump 42 can be used for vacuuming. At this time, the stable air pressure after one cycle is the limit air pressure pumped by the second mechanical pump 42. If a carrier gas is used in the coating process, the stable air pressure after one cycle is the equilibrium air pressure after the carrier gas is introduced;

[0108] During the coating process of the workpiece, the third telescopic support 34 or the fourth telescopic support 35 on the second sample stage 28 is adjusted every 20 minutes to complete the replacement of the fulcrum of the workpiece to avoid the failure of film deposition at the fulcrum;

[0109] After the coating is completed, the heating of the second heating element 29 is stopped, and 30 sccm of Ar is continuously introduced into the second coating chamber to increase the cooling rate of the workpiece. After the workpiece is cooled to room temperature, Ar is introduced into the second coating chamber to atmospheric pressure, the workpiece is taken out of the furnace, and the entire coating process is completed.

[0110] The above are only preferred embodiments of the present application and are not intended to limit the present application. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present application shall be included in the protection scope of the present application. The above are only preferred implementations of the present application. It should be pointed out that for ordinary technicians in this technical field, several improvements and variations can be made without departing from the technical principles of the present application, and these improvements and variations should also be regarded as the protection scope of the present application.

Claims

1. A device for low-temperature nickel plating on the surface of a radioactive substrate, characterized in that: include: A cleaning box assembly (1), the cleaning box assembly (1) comprising a cleaning box body (2), a cleaning sample table (3), an ion source (4) and a cleaning vacuum pipeline (5), the cleaning box body (2) being provided with an ion cleaning chamber, the cleaning sample table (3) being arranged in the cleaning box body (2) for placing a workpiece, the ion source (4) being arranged on the top and side wall of the cleaning box body (2), and its output end being located in the ion cleaning chamber, and the cleaning vacuum pipeline (5) being connected to the cleaning box body (2); A coating box assembly (6), wherein a gate plate (7) is arranged between the coating box assembly (6) and the cleaning box assembly (1), wherein the coating box assembly (6) comprises a first box body (8) and a first air inlet pipe (9), wherein a first coating cavity is provided inside the first box body (8), wherein a water cooling layer is provided inside the first box body (8), wherein the first coating cavity is used for storing workpieces after being cleaned by the cleaning box assembly (1), and wherein the first air inlet pipe (9) is connected to the first box body (8) for supplying coating gas into the first box body (8).

2. The device for low-temperature nickel plating on the surface of a radioactive substrate according to claim 1, characterized in that: The coating box assembly (6) further comprises a first sample stage (10), wherein the first sample stage (10) is arranged in the first coating chamber, and the first sample stage (10) is used for placing a workpiece.

3. The device for low-temperature nickel plating on the surface of a radioactive substrate according to claim 2, characterized in that: The first sample stage (10) comprises: A first supporting platform (11), wherein the first supporting platform (11) is disposed in the first coating chamber; A first telescopic support (12), wherein the first telescopic support (12) is symmetrically arranged on the first supporting platform (11); A second telescopic support (13), wherein the second telescopic support (13) is symmetrically arranged on the first support platform (11) and is located outside the first telescopic support (12), and the length of the second telescopic support (13) is greater than the length of the first telescopic support (12).

4. The device for low-temperature nickel plating on the surface of a radioactive substrate according to claim 3, characterized in that: The coating box assembly (6) also includes a first heating element (14), which includes an induction heating source (15) and an induction coil (16). The induction heating source (15) is arranged on the top of the first box body (8), and the induction coil (16) is connected to the induction heating source (15) for heating the workpiece.

5. The device for low-temperature nickel plating on the surface of a radioactive substrate according to claim 4, characterized in that: The coating box assembly (6) further comprises a first vacuum pumping pipeline (17), wherein the first vacuum pumping pipeline (17) is connected to the coating box assembly (6), and the first vacuum pumping pipeline (17) comprises: A first main pipeline (18), the first main pipeline (18) being connected to the coating box assembly (6), and the first main pipeline (18) being provided with a first valve (19), a first vacuum gauge (20), a second valve (21), a first molecular pump (22), a third valve (23) and a first mechanical pump (24) in sequence; A first branch pipeline (25), wherein a first end of the first branch pipeline (25) is connected to the first main pipeline (18) and is located between the second valve (21) and the first molecular pump (22); a second end of the first branch pipeline (25) is connected to the first main pipeline (18) and is located between the third valve (23) and the first mechanical pump (24); and a fourth valve (26) is provided on the first branch pipeline (25).

6. The device for low-temperature nickel plating on the surface of a radioactive substrate according to claim 1, characterized in that: The coating box assembly (6) comprises: A second box (27), wherein a second coating cavity is provided in the second box (27), and a heating layer is provided on the outside of the second box (27); A second sample table (28), the second sample table (28) is arranged in the second coating chamber and is used to place the workpiece after being cleaned by the cleaning box assembly (1); A second heating element (29), the second heating element (29) is symmetrically arranged in the second coating chamber and located on both sides of the second sample stage (28); A plasma source (30), the plasma source (30) being arranged on the top of the second box (27); A second air inlet pipeline (31), the second air inlet pipeline (31) being connected to the second box (27) and being used to supply coating gas into the interior of the first box (8); The second vacuum extraction pipeline (32) is connected to the second box (27).

7. The device for low-temperature nickel plating on the surface of a radioactive substrate according to claim 6, characterized in that: The second sample stage (28) comprises: A second supporting platform (33), wherein the second supporting platform (33) is disposed in the second coating chamber; A third telescopic support (34), wherein the third telescopic support (34) is symmetrically arranged on the second support platform (33); A fourth telescopic support (35), the fourth telescopic support (35) is symmetrically arranged on the second support platform (33) and is located outside the third telescopic support (34), and the length of the fourth telescopic support (35) is greater than the length of the third telescopic support (34).

8. The device for low-temperature nickel plating on the surface of a radioactive substrate according to claim 7, characterized in that: The second vacuum pumping pipeline (32) comprises: a second main pipe (36), the second main pipe (36) being connected to the second housing (27), and the second main pipe (36) being provided with a fifth valve (37), a second vacuum gauge (38), a sixth valve (39), a second molecular pump (40), a seventh valve (41) and a second mechanical pump (42) in sequence; A second branch pipeline (43), wherein a first end of the second branch pipeline (43) is connected to the second main pipeline (36) and is located between the fifth valve (37) and the second molecular pump (40); a second end of the second branch pipeline (43) is connected to the second main pipeline (36) and is located between the sixth valve (39) and the second mechanical pump (42); and an eighth valve (44) is provided on the second branch pipeline (43).

9. The device for low-temperature nickel plating on the surface of a radioactive substrate according to claim 1, characterized in that: The cleaning box (2) is provided with a transmission component (45).

10. A method for low-temperature nickel plating on a radioactive substrate surface, characterized in that: The device for low-temperature nickel plating on the surface of a radioactive substrate according to any one of claims 1 to 9 comprises the following steps: S1, placing a workpiece on the cleaning sample table (3) in the cleaning box assembly (1) to clean the sample; S2. Put the cleaned workpiece into the coating box assembly (6), and introduce coating gas into the coating box assembly (6) to coat the workpiece.

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