Sample degassing device and application thereof

Abstract

The invention provides a sample degassing device, and belongs to the technical field of degassing devices. The device comprises a cylindrical vacuum cavity, the two ends of the cylindrical vacuum cavity are sealed through a door and a vacuum feed-through to form the vacuum cavity, and the vacuum feed-through is used for transmitting signals; the annular cooling fin is arranged outside the cylindrical vacuum cavity and is used for cooling the cylindrical vacuum cavity; the vacuumizing device is used for vacuumizing the cylindrical vacuum cavity; and the heating device is arranged in the cylindrical vacuum cavity, is provided with a to-be-degassed article, and is used for heating the to-be-degassed article. The cylindrical vacuum cavity is matched with the annular cooling fins, so that the heat dissipation speed is increased, the heat dissipation time is shortened, and the heat dissipation efficiency is improved.

Description

Technical Field

[0001] The invention relates to the technical field of degassing devices, in particular to a sample degassing device and application thereof in degassing of radial objects. Background Art

[0002] The principle of vacuum heating baking degassing method is to use high temperature and vacuum environment to make the gas molecules in the material evaporate from the material. Under high vacuum conditions, the collision between gas molecules is almost negligible, so the gas molecules can easily evaporate from the surface of the material. At the same time, heating the material can increase the function of the gas molecules, making it easier to detach from the material. In this way, the gas content in the material can be reduced to an extremely low level, thereby obtaining a high-purity sample.

[0003] The high vacuum heating baking degassing method has several steps. The material to be processed is placed on the sample holder and then the holder is placed in the vacuum chamber as a whole. The gas in the chamber is extracted by a vacuum mechanical pump and a molecular pump until the required vacuum value is reached. The sample is heated. Through the rhenium belt heating process, the residual gas on the surface of the sample will gradually evaporate. At the same time, the mechanical pump and molecular pump will extract the evaporated gas out of the chamber to obtain a high-purity sample.

[0004] The vacuum heating baking degassing method also requires some key factors in practical application, such as the selection of parameters such as heating current and voltage, heating time, and vacuum degree, which are determined according to the characteristics and process requirements of the sample, and finally a material that meets the requirements is obtained.

[0005] In a vacuum state, there is no heat transfer through air molecules, and objects can only dissipate heat through thermal radiation. Therefore, the larger the surface area of ​​an object, the faster the heat dissipation speed and the faster the temperature drops; the material and thickness of the object will also affect the heat dissipation speed. Materials with high thermal conductivity dissipate heat faster, and the thinner the thickness, the faster the heat dissipation speed.

[0006] After prolonged heating, the terminals installed with the rhenium tape bracket will fail and the terminal accessories need to be replaced: After the sample is degassed, the heat dissipation is relatively slow because there is no gas to conduct heat in a vacuum environment. At the same time, thermal radiation will also be restricted, resulting in the heat not being effectively dissipated. Summary of the invention

[0007] In view of this, in order to solve the technical problem of slow heat dissipation of the existing degassing device, on the one hand, the present invention provides a sample degassing device, which adopts a cylindrical vacuum cavity with an annular heat sink to accelerate the heat dissipation speed, shorten the heat dissipation time, and improve the heat dissipation efficiency.

[0008] To achieve the above object, the present invention provides the following technical solutions: A sample degassing device, comprising: A cylindrical vacuum cavity, both ends of which are closed by doors and vacuum feedthroughs to form a vacuum cavity, wherein the vacuum feedthroughs are used to transmit signals; an annular heat sink, which is arranged outside the cylindrical vacuum cavity and is used to dissipate heat from the cylindrical vacuum cavity; A vacuum pumping device, used for vacuuming the cylindrical vacuum chamber; The heating device is arranged in the cylindrical vacuum chamber, on which the object to be degassed is arranged, and is used to heat the object to be degassed.

[0009] Preferably, it also includes: A controller is used to control the vacuum degree of the cylindrical vacuum chamber through the vacuum pumping device and to control the heating device to heat the object to be degassed.

[0010] Preferably, it also includes: A resistance gauge, used to measure the vacuum degree of the cylindrical vacuum chamber and transmit the measurement to the controller, and the controller controls the vacuum pumping device according to the vacuum degree; The BA gauge is used to measure the high vacuum degree and high temperature vacuum measurement of the cylindrical vacuum cavity and transmit the measurement to the controller, and the controller controls the vacuum pumping device according to the vacuum degree.

[0011] Preferably, it also includes: An air filling valve is used to fill the cylindrical vacuum chamber with air.

[0012] Preferably, it also includes: A multi-layer sample holder, which is arranged in the cylindrical vacuum chamber; A sample tray, used for being placed on the sample holder; A bracket, on which the heating device is arranged, is used for being installed on the sample tray.

[0013] Preferably, the vacuum pump is a molecular pump.

[0014] Preferably, the heating device is a rhenium belt, and the controller is used to control the heating temperature of the rhenium belt.

[0015] Preferably, an observation window is provided on the door.

[0016] Preferably, the door is locked by a plum blossom hand wheel locking mechanism.

[0017] On the other hand, the present invention also provides the application of the above-mentioned sample degassing device in the degassing of radioactive samples (for example: uranium, neodymium, rhenium, lithium, etc.).

[0018] Compared with the prior art, the present invention has the following beneficial effects: The sample degassing device provided by the present invention uses a cylindrical vacuum cavity with an annular heat sink to accelerate the heat dissipation speed, shorten the heat dissipation time, and improve the heat dissipation efficiency. Specifically: The cylindrical vacuum cavity has a high heat dissipation area, a compact structure, a uniform structure, high compressive strength, and simple processing. The addition of an annular heat sink to dissipate heat from the cylindrical vacuum cavity can greatly increase the heat dissipation area, speed up the heat dissipation speed, shorten the heat dissipation time, and improve the heat dissipation efficiency.

[0019] The present invention measures the front-stage vacuum degree by a resistance gauge and the chamber ultra-high vacuum degree by a BA gauge, and performs intelligent and automatic control through a controller, which greatly improves the convenience of operation and realizes intelligent and automatic management of the items to be degassed.

[0020] The degassing device provided by the present invention is safe, easy to use and convenient to operate. The items to be degassed are placed in a vacuum environment, and the protective cover can protect the cylindrical vacuum chamber from contamination. It is suitable for a variety of usage scenarios, especially the degassing operation of radioactive samples. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 A perspective view of the present invention; Figure 2 A three-dimensional diagram of the present invention with a protective cover; In the figure, 1. main frame; 2. cylindrical vacuum chamber; 3. annular heat sink; 4. molecular pump; 5. sample holder; 6. sample tray; 7. observation window; 8. vacuum feedthrough; 9. resistance gauge; 10. BA gauge; 11. inflation valve; 12. plum blossom handwheel locking mechanism; 13. protective cover; 14. controller. DETAILED DESCRIPTION

[0022] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention; it is obvious that the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments, and all other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making creative work are within the scope of protection of the present invention.

[0023] In the description of the present invention, it should be noted that the terms "upper", "lower", "inside", "outside", "top / bottom" and the like indicate orientations or positional relationships 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, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0024] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "provided with", "mounted / connected", "connected", etc. should be understood in a broad sense. For example, "connected" 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 indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0025] like Figure 1-2 As shown, the present invention provides a sample degassing device, comprising: A cylindrical vacuum cavity is closed at both ends by a door and a vacuum feedthrough (preferably a knife-edge flange is used to connect the vacuum feedthrough) to form a vacuum cavity, and the vacuum feedthrough is used to transmit signals. Vacuum feedthrough is a term in electronic engineering and physics, which is mainly used to describe a technology or component that transmits signals or energy in a vacuum environment. In a vacuum environment, since there are no traditional wires or cables to transmit signals, special devices are required to achieve signal transmission. Vacuum feedthrough is a general term for such special devices. Therefore, the vacuum feedthrough can be selected as known to those skilled in the art.

[0026] An annular heat sink is arranged outside the cylindrical vacuum cavity and is used for dissipating heat from the cylindrical vacuum cavity.

[0027] The present invention can increase the heat dissipation area by setting the vacuum cavity to be cylindrical, and the cylindrical vacuum cavity has a compact structure, uniform structure, high compressive strength and simple processing. The cylindrical vacuum cavity is cooled by an annular heat sink, which can greatly increase the heat dissipation area, speed up the heat dissipation speed, shorten the heat dissipation time and improve the heat dissipation efficiency.

[0028] A vacuum pump is used to vacuum the cylindrical vacuum chamber. In this technical solution, the vacuum pump can be a conventional vacuum pump in the present invention, and there is no special requirement for this. In the present invention, a molecular pump is preferably used, and the molecular pump is preferably connected to the cylindrical vacuum chamber through a knife-edge flange.

[0029] The heating device is arranged in the cylindrical vacuum chamber, and the object to be degassed is arranged on the heating device, and is used to heat the object to be degassed. The heating device is used to heat the object to be degassed, and any conventional heating device in the art can be selected.

[0030] The present invention also includes: The controller is used to control the vacuum degree of the cylindrical vacuum chamber through the vacuum pump and to control the heating device to heat the object to be degassed. The setting of the controller makes the present invention intelligent and automated, and can realize automated operation and intelligent management.

[0031] The present invention also includes: A resistance gauge, used to measure the vacuum degree of the cylindrical vacuum chamber and transmit the measurement to the controller, and the controller controls the vacuum pumping device according to the vacuum degree; BA gauge, used to measure the high vacuum degree and high temperature vacuum measurement of the cylindrical vacuum cavity, and transmit it to the controller, and the controller controls the vacuum pumping device according to the vacuum degree; Among them, the resistance gauge is used to measure the vacuum degree of the cylindrical vacuum cavity and transmit it to the controller. The controller controls the vacuum pumping device according to the vacuum degree; the key step of starting the molecular pump after the vacuum degree reaches the specified value realizes automatic control.

[0032] The present invention also includes: The inflation valve is used to inflate the cylindrical vacuum chamber. After the operation is completed, the vacuum is broken and the air is inflated through the inflation valve.

[0033] The present invention also includes: A multi-layer sample holder is arranged in the cylindrical vacuum chamber; preferably, it has two layers, upper and lower, which can hold two sample trays and a maximum of 48 samples.

[0034] A sample tray is used to be placed on the sample holder.

[0035] A bracket, on which the heating device is arranged, is used for being installed on the sample tray.

[0036] In the present invention, the heating device is a rhenium belt, and the controller is used to control the heating temperature of the rhenium belt. The object to be degassed is spot welded on the rhenium belt, and the controller controls the current and voltage of the rhenium belt to heat and degas quickly in a vacuum by using the rhenium belt. After the rhenium belt is heated, the temperature is controlled to about room temperature to more than one thousand degrees, and 1-48 samples are baked at a time.

[0037] In the present invention, an observation window is provided on the door, which is convenient for observing the state of the object to be degassed. The door and the observation window constitute a sample taking and placing structure, and the placing and taking out of the object is achieved by opening and closing the door.

[0038] In the present invention, the door is locked by a plum blossom handwheel locking mechanism. The plum blossom handwheel locking mechanism is a mechanism for fixing and locking the plum blossom handwheel to ensure the stability of the position of the handwheel and prevent it from accidentally rotating or moving. A suitable plum blossom handwheel locking mechanism can be selected according to actual needs.

[0039] In the present invention, a protective cover is also provided to cover the vacuum device to provide protection.

[0040] The molecular pump, cylindrical vacuum chamber and other components of the present invention are all arranged on the main frame.

[0041] On the other hand, the present invention also provides the application of the above sample degassing device in degassing radioactive samples, wherein the radioactive samples are preferably uranium, neodymium, rhenium, lithium and the like.

[0042] The workflow of the present invention is as follows: Spot weld the object to be degassed on the rhenium belt of the bracket, install the bracket into the fixing hole corresponding to the sample tray, put the sample tray into the sample holder, push it to the deepest part to connect the banana head, the sample holder is divided into two layers, two sample trays can be placed, and a maximum of 48 samples can be placed. Close the observation window, tighten it with the plum blossom handwheel locking mechanism, operate the controller to control the molecular pump to start extracting the internal air, and start controlling the temperature of the rhenium belt to heat the object to be degassed to degas.

[0043] The controller adjusts the working efficiency of the molecular pump and the heating temperature of the rhenium belt in real time according to the vacuum information fed back by the resistance gauge and the ultra-high vacuum measured by the BA gauge to ensure stable temperature and vacuum.

[0044] The above are only preferred specific implementations of the present invention; however, the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical solutions and improved concepts of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A sample degassing device, characterized in that: include: A cylindrical vacuum cavity, both ends of which are closed by doors and vacuum feedthroughs to form a vacuum cavity, wherein the vacuum feedthroughs are used to transmit signals; an annular heat sink, which is arranged outside the cylindrical vacuum cavity and is used to dissipate heat from the cylindrical vacuum cavity; A vacuum pumping device, used for vacuuming the cylindrical vacuum chamber; The heating device is arranged in the cylindrical vacuum chamber, on which the object to be degassed is arranged, and is used to heat the object to be degassed.

2. A sample degassing device according to claim 1, characterized in that: Also includes: A controller is used to control the vacuum degree of the cylindrical vacuum chamber through the vacuum pumping device and to control the heating device to heat the object to be degassed.

3. A sample degassing device according to claim 2, characterized in that: Also includes: A resistance gauge, used to measure the vacuum degree of the cylindrical vacuum chamber and transmit the measurement to the controller, and the controller controls the vacuum pumping device according to the vacuum degree; The BA gauge is used to measure the high vacuum degree and high temperature vacuum measurement of the cylindrical vacuum cavity and transmit the results to the controller, and the controller controls the vacuum pumping device according to the vacuum degree.

4. A sample degassing device according to claim 1, characterized in that: Also includes: An air filling valve is used to fill the cylindrical vacuum chamber with air.

5. A sample degassing device according to claim 1, characterized in that: Also includes: A multi-layer sample holder, which is arranged in the cylindrical vacuum chamber; A sample tray, used for being placed on the sample holder; A bracket, on which the heating device is arranged, is used for being installed on the sample tray.

6. A sample degassing device according to claim 1, characterized in that: The vacuum pump is a molecular pump.

7. A sample degassing device according to claim 2, characterized in that: The heating device is a rhenium belt, and the controller is used to control the heating temperature of the rhenium belt.

8. A sample degassing device according to claim 1, characterized in that: The door is provided with an observation window.

9. A sample degassing device according to any one of claims 1 to 8, characterized in that: The door is locked by a plum blossom hand wheel locking mechanism.

10. Use of the sample degassing device according to any one of claims 1 to 9 in degassing radioactive samples.

Images