A high-temperature and high-pressure air intake system to avoid oxidation of titanium film

Abstract

The present invention provides a high-temperature and high-pressure aspiration system for preventing titanium film oxidation, which relates to the technical field of application of compact deuterium-deuterium accelerator neutron source in neutron measurement and irradiation. A high vacuum pumping unit is used to vacuum the film preparation chamber and the film aspiration chamber, so as to achieve a 10 ‑5 Pa-level high vacuum is achieved; a micron-level high-purity titanium film is then prepared in a film preparation chamber using magnetron sputtering technology. After the titanium film is prepared, a magnetic rod transmission device is used to transport the titanium film sample into a film aspiration chamber in a high vacuum environment, where it is heated and raised in the high vacuum environment. A gate valve isolation device is then used to isolate the film aspiration chamber from the film preparation chamber, and high-purity, high-pressure gas is filled into the film aspiration chamber, ultimately achieving high-temperature, high-pressure gas adsorption on the titanium film under oxidation-free conditions. This method reduces the impact of the oxide layer on the metal film surface on gas adsorption.

Description

Technical Field

[0001] The invention relates to the technical field of application of a compact deuterium-deuterium accelerator neutron source in neutron measurement and irradiation, and mainly relates to a high-temperature and high-pressure air intake system for preventing titanium film oxidation. Background Art

[0002] Neutrons, due to their unique electrical neutrality, strong penetrating properties, and broad wavelength, have found widespread application in materials analysis, photography, oil well logging, food processing, and online neutron activation analysis. In compact deuterium-deuterium accelerator neutron generators, the characteristics of the deuterium target are crucial factors, with its lifetime and performance determining the overall performance of the neutron generator. The deuterium target consists of a substrate and a target membrane. The continuous bombardment of the deuterium ion beam in the accelerator generates significant heat. When the target temperature exceeds a certain level, deuterium gas adsorbed in the target membrane is released, reducing the neutron yield of the deuterium-deuterium reaction. Therefore, chromium-zirconium-copper or oxygen-free copper, with excellent thermal conductivity, is used as the substrate material for the deuterium target, and a cooling water circuit is provided to actively cool the target. Secondly, titanium, with its exceptionally high hydrogen / deuterium adsorption density and low atomic number, can adsorb up to 2 mol of hydrogen per 1 mol of titanium, making it a major focus of research in deuterium target membranes in recent years. Factors such as the deuterium target preparation process, target film thickness, and materials all affect neutron yield. Producing a high-performance deuterium target is crucial for a neutron generator. There are two main types of deuterium targets: an adsorption target, which uses titanium or other metal films as a carrier for deuterium gas. This involves naturally adsorbing deuterium gas under high temperature and high pressure conditions after the metal film is prepared. The other type of target is a self-contained target, which is formed by coating a titanium film or welding a titanium sheet onto the target substrate. The target is then bombarded with an active deuterium ion beam in the accelerator, continuously depositing deuterium particles within the film or sheet to form a self-contained deuterium target. High-purity titanium films are easily oxidized in air, forming a dense oxide layer on the surface. This oxide layer directly affects the titanium film's adsorption of deuterium particles, reducing the deuterium particle enrichment within the titanium film. This, in turn, affects the neutron yield during accelerator neutron experiments and the performance of the accelerator. Furthermore, the adsorption of deuterium particles by high-purity titanium films requires high temperature and high pressure, so the titanium film must be completely isolated from the air to prevent air contamination. Based on this, the present invention designs a high-temperature, high-pressure air intake system for titanium thin films to prevent oxidation. This effectively isolates the titanium film from air and then allows for high-temperature, high-pressure adsorption of deuterium particles, thereby increasing the deuterium particle enrichment within the titanium film. This is of great significance for improving the neutron yield of compact deuterium-deuterium accelerator neutron generators. Summary of the Invention

[0003] In order to solve the above technical problems, the present invention provides a high-temperature and high-pressure aspiration system that avoids oxidation of titanium thin films. It can realize high-temperature and high-pressure gas adsorption without contact with air after the sample is plated with titanium thin films, avoid the influence of the oxide layer on the surface of the titanium thin film on the adsorption of deuterium particles, and improve the enrichment of deuterium particles in the titanium thin film.

[0004] The present invention is achieved through the following technical solutions:

[0005] A high-temperature and high-pressure air suction system for preventing oxidation of titanium thin film comprises a thin film preparation chamber, a thin film air suction chamber, a gate valve isolation device, a magnetic rod transmission device, a high-temperature heating platform, and a high-vacuum exhaust unit; the thin film preparation chamber comprises a magnetron sputtering source, a plasma cleaning source and a second sample stage to realize the preparation of micron-level titanium thin film; the thin film air suction chamber is connected to the thin film preparation chamber, comprises a deuterium gas filling port, a deuterium gas discharge port and a first sample stage; the gate valve isolation device is located between the thin film preparation chamber and the thin film air suction chamber, and is used to vacuum-isolate the thin film preparation chamber and the thin film air suction chamber; the magnetic rod transmission device is located on the right side of the thin film preparation chamber, and is used to transfer the prepared titanium film to the thin film air suction chamber under a high vacuum environment; the high-temperature heating platform performs high-temperature heating on the first sample stage of the thin film air suction chamber; the high-vacuum exhaust unit is directly connected to the thin film preparation chamber, and provides a high vacuum environment for the thin film preparation chamber and the thin film air suction chamber.

[0006] Furthermore, the thin film preparation chamber is a stainless steel cube chamber with dimensions of 750×550×520 mm. It contains a magnetron sputtering source with a diameter of 75 mm, a plasma cleaning source with a diameter of 75 mm, and a second sample stage with a diameter of 150 mm. It can realize magnetron sputtering film preparation on the sample surface and effectively remove pollutants such as the oxide layer and adsorbed gas on the sample surface.

[0007] Furthermore, the film aspiration chamber is a stainless steel cube chamber with dimensions of 350×250×350 mm, which is connected to the film preparation chamber and contains a deuterium gas filling port, a deuterium gas discharge port and a first sample stage, which can realize high-temperature and high-pressure gas adsorption of the film sample that needs to be aspirated.

[0008] Furthermore, the diameter of the gate valve isolation device is 150 mm, and the installation direction of its sealing surface is from the film suction chamber to the film preparation chamber. When the film suction chamber is subjected to a high-temperature and high-pressure gas adsorption experiment, the pressure in the film suction chamber will reach 0.2 MPa, which is much greater than 10 of the film preparation chamber. -5Pa vacuum environment, thereby creating a sufficient pressure differential on both sides of the gate valve isolation device, compacting the sealing ring of the gate valve isolation device and preventing gas leakage from the suction chamber. After the film is completed, the deuterium gas vent of the film suction chamber is used to reduce the pressure in the chamber to the same pressure as the film preparation chamber. Only then can the gate valve isolation device be opened and the sample can be removed using the magnetic rod transmission device.

[0009] Furthermore, the magnetic rod transmission device is a vacuum feed-in device that can move in a vacuum environment. It uses magnetic force to drive the guide rod forward and backward in the vacuum chamber, thereby transferring the titanium film prepared in the film preparation chamber to the film suction chamber.

[0010] Furthermore, the high-temperature and high-pressure aspiration system for preventing oxidation of titanium thin films is described, and the high-temperature heating platform is a stainless steel heating plate with a diameter of 150 mm prepared by winding armored heating wire, with a power of 1.8 kW. It is located in the center of the thin film aspiration chamber and is mainly used to raise the sample to a high-temperature environment of more than 500°C.

[0011] Furthermore, the high vacuum pumping unit includes a molecular pump and a mechanical pump. The molecular pump is directly connected to the film preparation chamber, has a diameter of 250 mm, and a pumping speed of up to 2300 L / s. The vacuum pumping unit can reduce the vacuum degree in the film preparation chamber and the film suction chamber to less than 5×10 -5 Pa.

[0012] The beneficial effects of the present invention are:

[0013] The present invention is a simple and effective method for preventing surface oxidation of freshly prepared titanium films. It can provide a technology for effectively preventing surface oxidation for films that need to adsorb gas in a high-temperature and high-pressure environment, reduce the influence of the film oxide layer on the inhalation, and increase the enrichment of gas particles in the film. It provides good preparation conditions for the adsorption target in a compact deuterium-deuterium neutron generator and meets higher requirements for neutron yield. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 This is a schematic diagram of the overall cross-sectional structure of a high-temperature and high-pressure air intake system for avoiding oxidation of titanium film according to the present invention.

[0015] In the figure, 1-deuterium gas discharge port; 2-thin film suction chamber; 3-deuterium gas filling port; 4-first sample stage; 5-high-temperature heating stage; 6-gate valve isolation device; 7-thin film preparation chamber; 8-plasma cleaning source; 9-second sample stage; 10-robotic arm; 11-magnetron sputtering source; 12-vacuum exhaust unit; 13-molecular pump; 14-mechanical pump; 15-magnetic rod transmission device. DETAILED DESCRIPTION

[0016] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely for the purpose of explaining the present invention and are not intended to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.

[0017] like Figure 1 As shown, a high-temperature, high-pressure aspiration system for preventing oxidation of titanium thin films according to the present invention comprises a thin film aspiration chamber 2, a thin film preparation chamber 7, a vacuum pumping unit 12, a magnetic rod transmission device 15, a gate valve isolation device 6, and a high-temperature heating platform 5. The thin film aspiration chamber 2 and the thin film preparation chamber 7 are connected via the gate valve isolation device 6; the vacuum pumping unit 12 is connected to the thin film preparation chamber 7; the magnetic rod transmission device 15 is located on the right side of the thin film preparation chamber 7 and is connected to the robot arm 10 via a vacuum feed-in method; the gate valve isolation device 6 is located between the thin film aspiration chamber 2 and the thin film preparation chamber 7. When opened, the vacuum pumping unit 12 can vacuum-pump the two vacuum chambers to obtain a high vacuum environment. When closed, it can provide a sealed environment for the thin film aspiration chamber 2. The high-temperature heating platform 5 is located inside the first sample stage 4 of the thin film aspiration chamber 2 and can provide a high-temperature environment for the sample.

[0018] The thin film preparation chamber 7 is a stainless steel cube chamber with dimensions of 750×550×520 mm. It contains a magnetron sputtering source 11 with a diameter of 75 mm, a plasma cleaning source 8 with a diameter of 75 mm, and a second sample stage 9 with a diameter of 150 mm. It can realize magnetron sputtering film preparation on the sample surface and effectively remove pollutants such as the oxide layer and adsorbed gas on the sample surface.

[0019] The film aspiration chamber 2 is a stainless steel cube chamber with dimensions of 350×250×350 mm. It is connected to the film preparation chamber 7 and contains a deuterium gas filling port 3, a deuterium gas discharge port 1 and a first sample stage 4, which can realize high-temperature and high-pressure gas adsorption of the film sample that needs to be aspirated.

[0020] The diameter of the gate valve isolation device 6 is 150 mm, and the installation direction of its sealing surface is from the film suction chamber 2 to the film preparation chamber 7. When the film suction chamber 2 performs a high-temperature and high-pressure gas adsorption experiment, the pressure in the film suction chamber 2 will reach 0.2 MPa, which is much greater than 10 of the film preparation chamber 7. -5Pa vacuum environment, thereby creating a sufficient pressure differential on both sides of the gate valve isolation device 6, compacting the gate valve sealing ring and preventing gas leakage from the suction chamber. After the film is completely sucked, the pressure in the chamber needs to be reduced to the same level as the film preparation chamber 7 using the vent port 1 of the film suction chamber 2 before the gate valve isolation device 6 can be opened and the sample can be removed using the magnetic rod transmission device 15.

[0021] The magnetic rod transmission device 15 is a vacuum feed-in device that can move in a vacuum environment. It uses magnetic force to drive the guide rod forward and backward in the vacuum chamber to transfer the titanium film prepared in the film preparation chamber to the film suction chamber.

[0022] The high temperature heating stage 5 is a stainless steel heating plate with a diameter of 150 mm and a power of 1.8 kW. It is located at the center of the film suction chamber 2 and is mainly used to increase the temperature of the sample to more than 500°C.

[0023] The high vacuum pumping unit 12 includes a molecular pump 13 and a mechanical pump 14. The molecular pump 13 is directly connected to the film preparation chamber 7, has a diameter of 250 mm, and a pumping speed of up to 2300 L / s. The vacuum pumping unit 12 can reduce the vacuum degree in the film preparation chamber 7 and the film suction chamber 2 to less than 5×10 -5 Pa.

[0024] The present invention first grinds, polishes, and ultrasonically cleans the sample to be prepared into a thin film, and then places it on the second sample stage 9 of the thin film preparation chamber 7. The gate valve isolation device 6 is opened, and the vacuum pump unit 12 is turned on to provide a high vacuum environment for the thin film preparation chamber 7 and the thin film suction chamber 2. When the vacuum inside the chamber reaches 10 -5After reaching the Pa level, a specific flow rate of argon gas is introduced into the film preparation chamber 7, and the plasma cleaning source 8 is activated to further clean the sample surface. After plasma cleaning is complete, the magnetron sputtering source 11 is activated to complete the titanium thin film deposition on the sample surface. After the titanium thin film deposition is complete, the film sample is transferred to the first sample stage 4 of the film aspiration chamber 2 using the magnetic rod transmission device 15. The high-temperature heating stage 5 is then activated to heat the sample under a high vacuum environment. When the sample temperature reaches the specified temperature and the film aspiration chamber 2 is in a high vacuum environment, the gate valve isolation device 6 is closed. The specified gas is then introduced into the film aspiration chamber 2, allowing the sample to adsorb the gas under a high-temperature, high-pressure environment. After the high-temperature heating stage 5 is stopped, the sample is allowed to cool naturally, completing the aspiration sample preparation. Finally, the deuterium gas vent 1 of the film aspiration chamber 2 is used to remove any residual gas from the chamber. When the pressures in the film aspiration chamber 2 and the film preparation chamber 7 are balanced, the gate valve isolation device 6 is opened, and the sample is returned to the film preparation chamber 7 using the magnetic rod transmission device 15 for removal. In this system, the thin film sample is always in a high vacuum environment during the process of gas adsorption, which can prevent the surface of the thin film sample from coming into contact with air and causing oxidation.

[0025] The present invention does not describe in detail parts that belong to the common knowledge of those skilled in the art. The above-described embodiments are merely descriptions of preferred embodiments of the present invention. The preferred embodiments do not describe all details in detail, nor do they limit the invention to the specific embodiments described. Without departing from the spirit of the present invention, various modifications and improvements made by those skilled in the art to the technical solution of the present invention should fall within the scope of protection defined by the claims of the present invention.

Claims

1. A high-temperature and high-pressure gettering system for preventing oxidation of titanium thin films, characterized by: It includes a thin film preparation chamber, a thin film suction chamber, a plug-in valve isolation device, a magnetic rod transmission device, a high-temperature heating table, and a high-vacuum exhaust unit; the thin film preparation chamber includes a magnetron sputtering source, a plasma cleaning source and a second sample table to realize the preparation of micron-level titanium thin films; the thin film suction chamber is connected to the thin film preparation chamber, and includes a deuterium gas filling port, a deuterium gas discharge port and a first sample table; the plug-in valve isolation device is located between the thin film preparation chamber and the thin film suction chamber, and is used to vacuum-isolate the thin film preparation chamber and the thin film suction chamber; the magnetic rod transmission device is located on the right side of the thin film preparation chamber, and is used to transfer the prepared titanium film to the thin film suction chamber under a high vacuum environment; the high-temperature heating table performs high-temperature heating on the first sample table of the thin film suction chamber; the high-vacuum exhaust unit is directly connected to the thin film preparation chamber, and provides a high vacuum environment for the thin film preparation chamber and the thin film suction chamber.

2. The high-temperature and high-pressure gettering system for preventing titanium film oxidation according to claim 1, characterized in that: The film preparation chamber is a stainless steel chamber with a size of 750×550×520 mm, which contains a magnetron sputtering source with a diameter of 75 mm, a plasma cleaning source with a diameter of 75 mm, and a second sample stage with a diameter of 150 mm.

3. The high-temperature and high-pressure gettering system for preventing titanium film oxidation according to claim 1, characterized in that: The film suction chamber is a stainless steel chamber with dimensions of 350×250×350 mm.

4. The high-temperature and high-pressure gettering system for preventing titanium film oxidation according to claim 1, characterized in that: The diameter of the gate valve isolation device is 150 mm, and the installation direction of the sealing surface is from the film suction chamber to the film preparation chamber. When the film suction chamber is subjected to a high-temperature and high-pressure gas adsorption experiment, the pressure in the film suction chamber will reach 0.2 MPa, which is much greater than 10 of the film preparation chamber. -5 Pa vacuum environment, thereby forming a sufficient pressure difference on both sides of the gate valve isolation device, compacting the sealing ring of the gate valve isolation device, and preventing the gas in the film suction chamber from leaking out.

5. The high-temperature and high-pressure gettering system for preventing titanium film oxidation according to claim 1, characterized in that: The magnetic rod transmission device is a vacuum feed-in device that moves in a vacuum environment. It uses magnetic force to drive the guide rod forward and backward in the vacuum chamber, and transfers the titanium film prepared in the film preparation chamber to the film suction chamber.

6. The high-temperature and high-pressure gettering system for preventing titanium film oxidation according to claim 1, characterized in that: The high-temperature heating stage is a stainless steel heating plate with a diameter of 150 mm and a power of 1.8 kW. It is located in the center of the film suction chamber and provides a high-temperature environment of more than 500°C for the sample.

7. The high-temperature and high-pressure gettering system for preventing titanium film oxidation according to claim 2, characterized in that: The high vacuum pumping unit includes a molecular pump and a mechanical pump. The molecular pump is directly connected to the film preparation chamber, has a diameter of 250 mm, and a pumping speed of 2300 L / s. The vacuum pumping unit pumps the vacuum degree in the film preparation chamber and the film suction chamber to less than 5×10 -5 Pa.

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