Molecular sieve activation device and activation method for high-purity germanium detector under vacuum sealing condition

Abstract

The application provides a high-purity germanium detector molecular sieve activation device and activation method under vacuum sealing conditions, and is used for solving the technical problems of low efficiency, complicated operation and difficult process guarantee of the existing molecular sieve activation method, unstable adsorption performance and quality of the molecular sieve, poor adsorption effect and poor economy. The high-purity germanium detector molecular sieve activation device under vacuum sealing conditions comprises an automatic control unit formed by an alternating current contactor, a temperature controller and a starting button, and the automatic control unit is matched with a temperature sensor and a heating pipe respectively, so that the molecular sieve activation device has a temperature monitoring function, and automatic stopping and automatic heating of the molecular sieve heating activation are realized through temperature monitoring. The application has the advantages of simple structure, convenient control, molecular sieve activation and vacuum preservation functions, cost saving, activation efficiency improvement, high vacuum high-temperature baking and degassing functions of the vacuum assembly, and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to a molecular sieve activation device, in particular to a high-purity germanium detector molecular sieve activation device and activation method under vacuum sealing conditions. BACKGROUND

[0002] High-purity germanium (HPGe) detectors have been widely used in scientific research and industrial and agricultural production due to their high energy resolution, high detection efficiency, and stable performance. The germanium crystal of the HPGe detector needs to work in a high-vacuum and low-temperature environment. A low-temperature adsorbent is placed in the vacuum chamber of the HPGe detector to improve the vacuum degree of the vacuum chamber. Molecular sieve is a silicate compound with a cubic lattice, which has a uniform cavity-like cell microporous structure. The microporous structure forms a grid-like porous structure with windows between the cavity cells. Molecules with diameters smaller than the windows can be adsorbed on the inner surface of the cells through the windows. Molecular sieve has preferential adsorption capacity for polar molecules and unsaturated molecules. At liquid nitrogen temperature (77K), molecular sieve can adsorb 110 times the size of its own volume of gas, so it can make the original standard atmospheric pressure vacuum chamber achieve a vacuum degree of 1.33 Pa. Due to its high adsorption capacity and strong thermal stability, molecular sieve is often used as a low-temperature adsorbent to improve the vacuum degree of the vacuum chamber of the HPGe detector. The molecular sieve is installed between the first-stage amplification circuit and the base flange in the vacuum chamber of the HPGe detector, which facilitates the disassembly and replacement of the molecular sieve. At the same time, the molecular sieve is placed in the joint of the detachable cold finger of the HPGe detector vacuum chamber to ensure and maintain the vacuum degree of the cold finger at low temperature.

[0003] When using molecular sieve as a low-temperature adsorbent for HPGe detectors, it is necessary to note that when the molecular sieve adsorbs a large amount of water vapor in the atmosphere, its adsorption capacity will be greatly reduced, and it is generally required that the water content should not exceed 2%. In use, the molecular sieve should be avoided from being exposed to the atmosphere, because the molecular sieve can absorb more than 2% of the water in a few hours in the atmosphere. When the water and other substances adsorbed by the molecular sieve reach saturation, the molecular sieve will fail, which will destroy the vacuum degree in the vacuum chamber of the HPGe detector, directly leading to a decrease in its adiabatic performance. When the molecular sieve fails, it needs to be baked in a vacuum environment to remove the water and other substances inside the molecular sieve, restoring the adsorption performance of the adsorption centers on the surface of the molecular sieve, which is the activation of the molecular sieve.

[0004] When the HPGe detector is opened for maintenance, the molecular sieve is exposed to the ambient atmosphere, which causes saturation failure. After long-term use, the adsorption performance of the molecular sieve will decrease until saturation failure due to the outgassing of the surface of the molecular sieve and other substances adsorbed in the vacuum chamber. Since the temperature (60-120℃) of the HPGe detector during high-vacuum heat treatment is much lower than the activation temperature of the molecular sieve (-350℃), the saturated molecular sieve cannot be effectively activated, which causes the adsorbed water and gas and other substances to be unable to be completely removed, thereby affecting the low-temperature adsorption performance and further reducing the energy resolution of the HPGe detector. In addition, the internal components of the newly designed and processed vacuum chamber of the HPGe detector also need to be packaged and high-vacuum high-temperature baked to remove the adsorbed substances on the surface and reduce the surface outgassing. Since the purity of the germanium crystal in the vacuum chamber of the HPGe detector is extremely high (99.9999999999%-99.99999999999%), when the germanium crystal surface adsorbs other impurity substances, it will seriously affect the surface state of the crystal, cause dark current noise, and cause the energy resolution and other performance indicators of the HPGe detector to decrease seriously. Therefore, for the molecular sieve used as the low-temperature adsorbent of the HPGe detector, not only the adsorbed water vapor needs to be removed during activation, but also other adsorbed substances need to be removed efficiently, and the molecular sieve should not adsorb other impurity substances during the activation process. The adsorbed water vapor and other substances need to be extracted through a high-vacuum system during high-temperature activation, so that the molecular sieve is efficiently activated and high-vacuum purified. Therefore, a vacuum sealing device for activating the molecular sieve of the high-purity germanium detector needs to be designed to achieve high-temperature high-vacuum activation of the saturated molecular sieve.

[0005] Chinese patent CN 206027728 U discloses a molecular sieve activation regeneration device, the device mainly includes a nitrogen source, a support and a heater, the technical scheme can remove the residual gas and moisture in the cylindrical molecular sieve container through the nitrogen source, which helps to activate the molecular sieve. However, since the cylindrical heating element is wrapped around the side wall of the cylindrical molecular sieve container, it is difficult to ensure that each molecular sieve is uniformly heated, resulting in unsatisfactory dehydration performance of the molecular sieve. Chinese patent CN 103316631 A discloses a molecular sieve activation treatment process, which mainly includes first heating and drying treatment, second heating and vacuumizing, third nitrogen charging and replacing, and fourth nitrogen charging and preserving processes. The molecular sieve is loaded in the activation tank during activation, and the activation tank is sleeved in the activation furnace, so it is also difficult to ensure that the molecular sieve in different parts of the activation tank is uniformly heated, and only vacuumizing is performed in the second process during the activation process. Therefore, it can be seen that the existing molecular sieve activation treatment process method is complicated and different, the principle and process are basically similar to the above-mentioned disclosure, and it is mainly used for the application of molecular sieve in the industrial field. The molecular sieve is heated to the activation temperature by high-temperature gas purging, but the specific heat capacity of the gas is small, and the heating efficiency is low. Moreover, the existing activation device cannot uniformly heat the molecular sieve during heating, cannot fully dry the molecular sieve, and cannot achieve excellent dehumidification efficiency and effect of the molecular sieve, so that the use effect of the molecular sieve is limited in the next use. In summary, the existing molecular sieve activation method has low efficiency, complex operation and difficult process, which leads to unstable adsorption performance and quality of the molecular sieve, poor adsorption effect and poor economy. SUMMARY

[0006] The purpose of the present application is to solve the technical problems of low efficiency, complex operation and difficult process of the existing molecular sieve activation method, which leads to unstable adsorption performance and quality of the molecular sieve, poor adsorption effect and poor economy, and to provide a high-purity germanium detector molecular sieve activation device and activation method under vacuum sealing conditions.

[0007] In order to achieve the above-mentioned purpose, the technical scheme provided by the present application is as follows:

[0008] A high-purity germanium detector molecular sieve activation device under vacuum sealing conditions, characterized in that it comprises a vacuum sealing unit, an activation unit, an automatic control unit and a temperature sensor.

[0009] The vacuum sealing unit comprises a vacuum activation container, and a first sealing adapter structure and two second sealing adapter structures sealingly arranged on the side wall of the vacuum activation container.

[0010] The activation unit comprises a heating pipe, a heating plate and an insulating support.

[0011] The heating plate is a hollow box structure, which is installed in the vacuum activation container through an insulating support; a plurality of activation recesses for placing molecular sieves are arranged on the upper surface of the top plate of the heating plate; and a hollow groove matched with the structure of the heating pipe is arranged in the heating plate, and the heating pipe is arranged in the hollow groove;

[0012] The automatic control unit comprises an AC contactor, a temperature controller and a start button; the AC contactor comprises an iron core and a KM coil wound on the iron core;

[0013] The A2 terminal of the KM coil is connected with the power supply N phase input port of the AC contactor, and the A1 terminal is connected with the output voltage L phase port of the temperature controller; the input voltage L phase port of the temperature controller is connected with the power supply L phase input port of the AC contactor through the start button; and the input voltage N phase port of the temperature controller is connected with the power supply N phase input port of the AC contactor;

[0014] The temperature sensor is installed on the top plate of the heating plate and used for monitoring the activation temperature of the molecular sieves in the activation recess, and the signal output positive terminal and the signal output negative terminal of the temperature sensor are connected with two inner terminal interfaces of the first sealed adapter structure; and two outer terminal interfaces of the first sealed adapter structure are respectively connected with the signal first input port and the signal second input port of the temperature controller;

[0015] The L phase output port and the N phase output port of the AC contactor are respectively connected with the outer terminal interfaces of two second sealed adapter structures, and the inner terminal interfaces of the two second sealed adapter structures are respectively connected with the power supply input L phase and the power supply input N phase of the heating pipe.

[0016] Further, the vacuum activation container comprises a stainless steel tank body with an open upper end and a flange sealing cover; the flange sealing cover is sealingly connected to the upper end of the stainless steel tank body through a hinge assembly;

[0017] An installation through hole is formed in the side wall of the stainless steel tank body, and the vacuum negative pressure gauge is installed outside the installation through hole;

[0018] A vacuum interface and a pressure relief valve are arranged on the side wall of the stainless steel tank body;

[0019] The first sealed adapter structure and the two second sealed adapter structures are sealingly connected to the side wall of the stainless steel tank body.

[0020] Further, the first sealed adapter structure comprises a vacuum adapter interface A, a vacuum adapter interface B, two first conductive bodies and a first clamp;

[0021] The vacuum adapter interface A is an integrated structure with the side wall of the stainless steel tank body, and two first threaded through holes are axially formed in the vacuum adapter interface A;

[0022] The vacuum adapter B comprises a first shell and two first sealing blind plates; two second threaded holes are axially formed on the first shell at positions corresponding to the two first threaded holes; the outer side walls of the two first conductive bodies are respectively provided with external threads for being threadedly connected with the corresponding second threaded holes and first threaded holes in sequence; the two first sealing blind plates are respectively sleeved on the corresponding first conductive bodies at positions connected with the first shell, so as to realize the fixed connection of the two first conductive bodies with the first shell;

[0023] The first clamp is arranged on the outer side wall of the first shell at the position where the vacuum adapter A is connected with the vacuum adapter B, so as to realize the fixed connection of the vacuum adapter A with the vacuum adapter B;

[0024] The intermediate part of the first conductive body is closed, and the two ends thereof are respectively axially provided with insertion holes; the insertion holes at the inner ends of the two first conductive bodies are respectively used as two inner end interfaces of the first sealing adapter structure, and the insertion holes at the outer ends thereof are respectively used as two outer end interfaces of the first sealing adapter structure;

[0025] The two second sealing adapter structures respectively comprise a vacuum adapter C, a vacuum adapter D, a second conductive body and a second clamp;

[0026] The vacuum adapter C is in an integrated structure with the side wall of the stainless steel tank body, and a third threaded hole is axially formed on the vacuum adapter C;

[0027] The vacuum adapter D comprises a second shell and a second sealing blind plate; a fourth threaded hole is axially formed on the second shell at a position corresponding to the third threaded hole; the outer side wall of one end of the second conductive body is provided with an external thread for being threadedly connected with the fourth threaded hole and the third threaded hole in sequence; and the second sealing blind plate is sleeved on the second conductive body at a position connected with the second shell, so as to realize the fixed connection of the second conductive body with the second shell;

[0028] The second clamp is arranged on the outer side wall of the second shell at the position where the vacuum adapter C is connected with the vacuum adapter D, so as to realize the fixed connection of the vacuum adapter C with the vacuum adapter D;

[0029] The intermediate part of the second conductive body is closed, and the two ends thereof are respectively axially provided with insertion holes; the insertion hole at the inner end of the second conductive body is used as an inner end interface of the second sealing adapter structure, and the insertion hole at the outer end thereof is used as an outer end interface of the second sealing adapter structure.

[0030] Further, the signal output positive terminal and the signal output negative terminal of the temperature sensor, the signal first input port and the signal second input port of the temperature controller, the L-phase output port and the N-phase output port of the alternating current contactor, and the terminal connection of the wires on the power input L-phase and the power input N-phase of the heating pipe are all arranged as banana plug structures made of copper plated with nickel;

[0031] The first conductor, the inner end and the outer end of the second conductor are all provided with high-conductivity oxygen-free copper jacks matched with banana plug structures, which are used for connecting with the corresponding banana plug structures.

[0032] The end face of the first shell towards the vacuum interface A and the end face of the second shell towards the vacuum interface C are respectively provided with grooves; each groove is provided with a fluororubber ring with a support, which is used for realizing the sealing connection of the corresponding interface.

[0033] Further, the vacuum interface, the vacuum adapter interface A and the vacuum adapter interface C are all KF40 vacuum interfaces made of stainless steel.

[0034] The vacuum adapter interface B and the vacuum adapter interface D are both KF40 vacuum interfaces made of polytetrafluoroethylene.

[0035] The insulating support is made of polyimide insulating material.

[0036] The heating pipe is O-shaped.

[0037] Further, the outer side wall of the insulating support is provided with an outer thread at the upper end, which is used for threaded connection with the bottom plate of the heating plate; the lower end of the insulating support is provided with a sharp structure, which is in contact with the upper surface of the bottom of the stainless steel tank body, so as to support the stainless steel tank body at the bottom and realize a small contact area.

[0038] Further, the temperature sensor is a Pt100 platinum resistance temperature sensor.

[0039] Further, the stainless steel tank body and the flange sealing cover are sealed by a first sealing ring.

[0040] The first conductor and the first shell are sealed by a second sealing ring.

[0041] The second conductor and the second shell are sealed by a third sealing ring.

[0042] Further, the stainless steel tank body and the flange sealing cover are both made of stainless steel; the size of the stainless steel tank body is with a wall thickness of 5mm, and the size of the flange sealing cover is

[0043] The size of the heating plate is The top plate of the heating plate is provided with 13 activation counterbores.

[0044] In addition, the application also provides an activation method of the high-purity germanium detector molecular sieve activation device under the vacuum sealing condition, and the special feature is that:

[0045] Step 1: Place the high-purity germanium detector molecular sieve in the activated sink on the heating plate;

[0046] Step 2: Connect the vacuum interface to the external vacuum pumping system and start the vacuum pumping system to perform high vacuum pumping;

[0047] Step 3: Connect the positive signal output terminal and the negative signal output terminal of the temperature sensor to the two inner end interfaces of the first sealed adapter structure, respectively, and connect the first signal input port and the second signal input port of the temperature controller to the two outer end interfaces of the first sealed adapter structure, respectively; at the same time, connect the L-phase output port and the N-phase output port of the AC contactor to the outer end interfaces of the two second sealed adapter structures, respectively, and connect the inner end interfaces of the two second sealed adapter structures to the L-phase power input and the N-phase power input of the heating tube, respectively;

[0048] Step 4: Connect a 220V power supply to the L-phase input port and the N-phase input port of the AC contactor, and manually press the start button to start heating the heating tube, thereby heating and activating the molecular sieve in the activated sink hole;

[0049] Step 5: The temperature sensor monitors the activation temperature of the molecular sieve in the activation sink. When the activation temperature is higher than the temperature threshold, the heating is automatically stopped. When the activation temperature is lower than the temperature threshold, the molecular sieve is automatically heated again for activation until the molecular sieve activation is completed.

[0050] The beneficial effects of the present invention compared to the prior art are as follows:

[0051] 1. The present invention provides a high-purity germanium detector molecular sieve activation device under vacuum sealing conditions, which forms an automatic control unit through an AC contactor, a temperature controller and a start button. The automatic control unit cooperates with the temperature sensor and the heating tube to enable the molecular sieve activation device to have a temperature monitoring function, and realizes automatic stopping and automatic heating of the molecular sieve heating activation by monitoring the temperature; the present invention has a simple structure and convenient control. It not only has the activation and vacuum preservation functions of batch molecular sieves, which can save operating costs and improve activation efficiency, but also has the high vacuum and high temperature baking and degassing function of the vacuum component.

[0052] 2. Aiming at the high vacuum and low temperature working environment of the germanium crystal of the high-purity germanium detector, the present invention has made special structural designs for the first sealing transition structure and the second sealing transition structure, which greatly improves the overall sealing vacuum performance of the device, so that the entire molecular sieve activation device can adapt to the high vacuum operating environment while realizing automatic control of temperature monitoring and molecular sieve heating activation.

[0053] 3. The present invention provides an activation method for a molecular sieve activation device for a high-purity germanium detector under vacuum sealing conditions, which has simple steps, convenient control, and high vacuum degree, and can be widely used in the molecular sieve activation of high-purity germanium detectors. BRIEF DESCRIPTION OF THE DRAWINGS

[0054] Figure 1 This is a schematic structural diagram of an embodiment of a high-purity germanium detector molecular sieve activation device under vacuum sealing conditions according to the present invention;

[0055] Figure 2 A top view of the vacuum activated container with the flange sealing cover open in an embodiment of the present invention;

[0056] Figure 3 This is a structural diagram of a first sealing transition structure in an embodiment of the present invention;

[0057] Figure 4 2 is a schematic structural diagram of a second sealing transition structure in an embodiment of the present invention;

[0058] Figure 5 This is a schematic structural diagram of the molecular sieve placed in the activation sink in the embodiment of step 1 of the activation method of the high-purity germanium detector molecular sieve activation device under vacuum sealing conditions of the present invention.

[0059] The specific reference numerals are as follows:

[0060] 0 - AC contactor; 1 - Power supply L-phase input port; 2 - Power supply N-phase input port; 3 - Start button; 4 - Iron core; 5 - KM coil; 6 - L-phase output port; 7 - N-phase output port; 8 - Input voltage N-phase port; 9 - Input voltage L-phase port; 10 - Output voltage L-phase port; 11 - Signal input port 1; 12 - Signal input port 2; 13 - Temperature controller;

[0061] 20 - Vacuum activated container; 21 - Flange sealing cover; 22 - Handle; 23 - Vacuum negative pressure gauge; 24 - First sealing ring; 25 - Hinge assembly; 26 - Stainless steel tank body; 27 - Pressure relief valve; 28 - Vacuum interface; 29 - First sealing transition structure; 30 - Second sealing transition structure;

[0062] 31-temperature sensor; 32-heating tube; 33-heating plate; 34-activated countersunk hole; 35-insulating bracket;

[0063] 40 - groove; 41 - first shell; 42 - first conductor; 43 - first sealing blind plate; 44 - socket; 45 - second shell; 46 - second conductor; 47 - second sealing blind plate; 48 - second sealing ring; 49 - third sealing ring. DETAILED DESCRIPTION

[0064] In order to make the advantages and features of the present application more clear, the present application is further described in detail below in combination with the drawings and specific embodiments.

[0065] As shown in Figure 1 , Figure 2 A kind of molecular sieve activation device of high purity germanium detector under vacuum sealing condition, it is applicable to the activation of molecular sieve in the vacuum chamber and cold finger joint of high purity germanium detector germanium crystal, it includes vacuum sealing unit, activation unit, automatic control unit and temperature sensor 31.

[0066] Vacuum sealing unit is used to realize the function of high vacuum sealing and molecular sieve vacuum preservation during the activation of molecular sieve. The vacuum sealing unit includes a vacuum activation container 20, a first sealing adapter structure 29 and two second sealing adapter structures 30. The vacuum activation container 20 includes a stainless steel tank body 26 with an open upper end and a flange sealing cover 21. The flange sealing cover 21 is sealingly connected to the upper end of the stainless steel tank body 26 through a hinge assembly 25, which facilitates the maintenance of the components inside the stainless steel tank body 26. The flange sealing cover 21 is a fixed bolt-free structure, which utilizes internal negative pressure and a first sealing ring 24 to achieve vacuum sealing between the stainless steel tank body 26 and the flange sealing cover 21. Both the stainless steel tank body 26 and the flange sealing cover 21 are made of stainless steel. In this embodiment, the size of the stainless steel tank body 26 is 5mm in wall thickness, and the size of the flange sealing cover 21 is

[0067] A mounting hole is formed in the side wall of the stainless steel tank body 26, and a vacuum negative pressure gauge 23 is installed outside the mounting hole for monitoring the negative pressure value inside the vacuum activation container 20. At the same time, the side wall of the stainless steel tank body 26 is also provided with a vacuum interface 28, a pressure relief valve 27 and a handle 22; the vacuum interface 28 is used to connect with an external vacuum pumping system for high vacuum pumping during the entire activation process of the molecular sieve. The external vacuum pumping system is composed of an oil-free mechanical pump, a molecular pump and a vacuum pipeline; the pressure relief valve 27 is a manual flap valve for internal pressure relief of the vacuum activation container 20.

[0068] The activation unit is used to realize the high-temperature activation function of the molecular sieve, and includes a heating plate 33, a heating pipe 32 and an insulating support 35. The heating plate 33 is a hollow box structure, which is enclosed by a top plate, a bottom plate and four side plates, and is connected by a countersunk screw. The insulating support 35 is placed on the inner bottom plate of the vacuum activation container 20, and the heating plate 33 is installed at the upper end of the insulating support 35. Since the polyimide has the properties of resisting 400℃ high temperature, tensile strength above 100 MPa, good dielectric performance, small thermal expansion coefficient, and small outgassing amount under extremely high vacuum, it meets the high-temperature and high-vacuum working environment during the activation process of the molecular sieve, and therefore the insulating support 35 is preferably made of polyimide for insulation support. Specifically, the outer side wall of the insulating support 35 is provided with an external thread at the upper end, which is used for threaded connection with the bottom plate of the heating plate 33, and the lower end is in contact with the upper surface of the bottom of the stainless steel tank body 26, so as to support the bottom of the stainless steel tank body 26. Preferably, the lower end of the insulating support 35 is provided in a sharp structure, which can effectively reduce the contact area between the insulating support 35 and the bottom of the stainless steel tank body 26, thereby reducing the heat loss during the activation of the molecular sieve.

[0069] The size of the heating plate 33 is The upper surface of the top plate is provided with thirteen activation countersunk holes 34 of Φ18mmx20mm, and each activation countersunk hole 34 is used to place the molecular sieve, and the batch activation of the molecular sieve is realized through the thirteen activation countersunk holes 34. At the same time, the inside of the heating plate 33 is provided with a hollow groove in the vertical direction, which is matched with the structure of the heating pipe 32, and the heating pipe 32 is placed in the hollow groove, which is used to transfer the heat of the heating pipe 32 to the heating plate 33. In this embodiment, the heating pipe 32 is preferably provided in an O shape, and correspondingly, the structure of the hollow groove is also in an O shape.

[0070] The automatic control unit is used to realize the automatic opening and closing function of the high-temperature activation of the molecular sieve, which is installed in a control box, so that the structure of the vacuum sealing unit is compact and the connection is convenient. The automatic control unit includes an AC contactor 0, a temperature controller 13 and a start button 3. The AC contactor 0 includes an iron core 4 and a KM coil 5 wound on the iron core 4, and is further provided with a power L-phase input port 1, a power N-phase input port 2, an L-phase output port 6 and an N-phase output port 7. The temperature controller 13 is provided with a temperature threshold value, and the temperature controller 13 is provided with an input voltage N-phase port 8, an input voltage L-phase port 9, an output voltage L-phase port 10, a signal first input port 11 and a signal second input port 12.

[0071] The A2 terminal of the KM coil 5 is connected with the power supply N phase input port 2 of the AC contactor 0, and the A1 terminal is connected with the output voltage L phase port 10 of the temperature controller 13; the input voltage L phase port 9 of the temperature controller 13 is connected with the power supply L phase input port 1 of the AC contactor 0 through the starting button 3; and the input voltage N phase port 8 of the temperature controller 13 is connected with the power supply N phase input port 2 of the AC contactor 0.

[0072] The temperature sensor 31 is installed on the top plate of the heating plate 33 and is used for monitoring the activation temperature of the molecular sieve in the activation counterbore 34. The signal output positive terminal and the signal output negative terminal of the temperature sensor 31 are respectively connected with the two inner end interfaces of the first sealed adapter structure 29, and the two outer end interfaces of the first sealed adapter structure 29 are respectively connected with the signal first input port 11 and the signal second input port 12 of the temperature controller 13. The temperature controller 13 is used for monitoring the temperature of the molecular sieve in the activation process through the signal input by the temperature sensor 31 and controlling the opening and closing circuit of the contact of the AC contactor 0 according to the monitored temperature. In the embodiment, the temperature sensor 31 is a Pt100 platinum resistance temperature sensor, and other temperature sensors can also be used in other embodiments of the application. The input of the power supply L phase input port 1 and the power supply N phase input port 2 is 220V voltage.

[0073] The L phase output port 6 of the AC contactor 0 and the N phase output port 7 of the AC contactor 0 are respectively connected with the outer end interface of one of the two second sealed adapter structures 30, and the inner end interfaces of the two second sealed adapter structures 30 are respectively connected with the power supply input L phase and the power supply input N phase of the heating tube 32, which are used for realizing the connection and disconnection of the working power supply of the O-shaped heating tube 32 through the opening and closing circuit of the contact of the AC contactor 0.

[0074] The working principle of the automatic control unit is that when the power supply L phase input port 1 and the power supply N phase input port 2 maintain 220V power supply, the output voltage L phase port 10 of the temperature controller 13 is connected, the KM coil 5 of the AC contactor 0 is powered, the electromagnetic attraction of the iron core 4 is generated, the contact is attracted and closed, so as to connect the power supply, the output voltage of the L phase output port 6 and the N phase output port 7 is connected, and the working power supply is provided to the heating tube 32. The heating tube 32 heats and transmits heat to the activation counterbore 34 in the heating plate 33, and the molecular sieve placed in the activation counterbore 34 starts high-temperature activation.

[0075] The temperature sensor 31 monitors the temperature in the activation hole 34. When the temperature monitored by the temperature sensor 31 is higher than a threshold value, the output voltage L-phase port 10 of the temperature controller 13 outputs a cut-off, the KM coil 5 is powered off, the electromagnetic attraction of the iron core 4 disappears, the contacts of the AC contactor 0 are disconnected, the voltage output is interrupted, the working power supply of the heating tube 32 is cut off, and the heating tube 32 stops working; when the temperature monitored by the temperature sensor 31 is lower than the threshold value, the output voltage L-phase port 10 of the temperature controller 13 is turned on again, the contacts of the AC contactor 0 are closed, the working power supply of the heating tube 32 is turned on again, and the molecular sieve placed in the activation hole 34 is activated at high temperature again.

[0076] Meanwhile, the first sealing adapter structure 29 and the second sealing adapter structure 30 are specially designed. As shown in Figure 3 The first sealing adapter structure 29 includes a vacuum adapter interface A, a vacuum adapter interface B, two first conductive bodies 42, and a first clamp. The vacuum adapter interface A is arranged on the stainless steel tank body 26 and is in an integrated structure with the side wall of the stainless steel tank body 26, and two first threaded through holes are axially arranged on the vacuum adapter interface A. The vacuum adapter interface B includes a first shell 41 and two first sealing blind plates 43. The first shell 41 is axially provided with two second threaded through holes corresponding to the positions of the two first threaded through holes, and the outer side walls of one ends of the two first conductive bodies 42 are respectively provided with external threads for being threadedly connected with the corresponding second threaded through holes and first threaded through holes in sequence. The two first sealing blind plates 43 are respectively arranged on the positions of the first shell 41 connected with the corresponding first conductive bodies 42, so as to realize the fixation of the two first conductive bodies 42 and the first shell 41. Meanwhile, the sealing between the first conductive bodies 42 and the first shell 41 is realized through the second sealing ring 48. The first clamp is arranged on the outer side wall of the position where the vacuum adapter interface A and the first shell 41 of the vacuum adapter interface B are connected, so as to realize the fixation of the vacuum adapter interface A and the vacuum adapter interface B. The end face of the first shell 41 facing the vacuum interface A is provided with a groove 40, and a fluorine rubber ring with a bracket is arranged in the groove 40, so as to realize the sealing of the interface between the vacuum adapter interface A and the first shell 41.

[0077] The middle of the first conductive body 42 is closed and the two ends are respectively axially provided with a jack 44; the jack 44 of the inner end of the two first conductive bodies 42 is respectively used as the two inner end interfaces of the first sealed adapter structure 29, and the jack 44 of the outer end is respectively used as the two outer end interfaces of the first sealed adapter structure 29. The signal output positive end and the signal output negative end of the temperature sensor 31, the signal first input port 11 and the signal second input port 12 of the temperature controller 13 are all banana plug structures made of copper plated nickel, the jack 44 of the inner end of the first conductive body 42 and the jack 44 of the outer end are both high-conductive oxygen-free copper jacks matched with the banana plug structure, and the banana plug structure made of copper plated nickel and the high-conductive oxygen-free copper jack are matched to realize the conduction of the connecting line. This connection is convenient and fast, and the conduction performance is excellent.

[0078] Since the voltage output by the L-phase output port 6 and the N-phase output port 7 of the alternating current contactor 0 is 220V high voltage, the sealed adapter structures corresponding to the L-phase output port 6 and the N-phase output port 7 are separately provided, that is, two second sealed adapter structures 30 are provided, which can effectively avoid short circuit of the two line contacts. As shown in Figure 4 The two second sealed adapter structures 30 are similar in structure to the first sealed adapter structure 29, and each includes a vacuum adapter interface C, a vacuum adapter interface D, a second conductive body 46 and a second clamp. The vacuum adapter interface C is an integrated structure with the side wall of the stainless steel tank body 26, and a third threaded hole is axially formed in the vacuum adapter interface C. The vacuum adapter interface D includes a second shell 45 and a second sealing blind plate 47, and the second shell 45 is axially provided with a fourth threaded hole at a position corresponding to the third threaded hole; one end of the second conductive body 46 is provided with an external thread, which is used for threaded connection with the fourth threaded hole and the third threaded hole in sequence; the second sealing blind plate 47 is sleeved on the second conductive body 46 at the position connected with the second shell 45, and is used for fixed connection of the second conductive body 46 and the second shell 45; meanwhile, the second conductive body 46 and the second shell 45 are sealed by the third sealing ring 49. The second clamp is arranged on the outer side wall of the position where the vacuum adapter interface C is connected with the second shell 45 of the vacuum adapter interface D, and is used for fixed connection of the vacuum adapter interface C and the vacuum adapter interface D; similarly, the end face of the second shell 45 facing the vacuum interface C is provided with a groove 40, and a fluorine rubber ring with a bracket is arranged in the groove 40, which is used for sealing the interface between the vacuum adapter interface C and the second shell 45.

[0079] The second conductor 46 is closed in the middle and has a plug hole 44 at each end. The plug hole 44 at the inner end of the second conductor 46 is the inner end interface of the second sealed adapter structure 30, and the plug hole 44 at the outer end is the outer end interface of the second sealed adapter structure 30. Similarly, the L-phase output port 6 and the N-phase output port 7 of the AC contactor 0, and the wiring terminals of the power input L-phase and the power input N-phase of the heating tube 32 are all banana plug structures made of copper plated with nickel. The plug holes 44 at the inner end and the outer end of the two second conductors 46 are high-conductivity oxygen-free copper plug holes matching the outer diameter of the banana plug structure, used to cooperate to realize the conduction of the connection circuit. Preferably, the vacuum interface 28, the vacuum adapter interface A, and the vacuum adapter interface C of the embodiment are all KF40 vacuum interfaces made of stainless steel, and the vacuum adapter interface B and the vacuum adapter interface D are both KF40 vacuum interfaces made of polytetrafluoroethylene.

[0080] The activation method of the high-purity germanium detector molecular sieve activation device under vacuum sealing conditions is further described in detail below.

[0081] Step 1, place the high-purity germanium detector molecular sieve shown in the activation counterbore 34 on the heating plate 33, and close the flange sealing cover 21. Figure 5

[0082] Step 2, connect the vacuum interface 28 with the external vacuum pumping system, and start the vacuum pumping system to perform high-vacuum pumping.

[0083] Step 3, insert the wiring terminals of the wires on the signal first input port 11 and the signal second input port 12 of the temperature controller 13 and the temperature sensor 31 into the plug holes 44 at the inner end and the outer end of the first conductor 42, respectively, and insert the wiring terminals of the wires on the L-phase output port 6 and the N-phase output port 7 of the AC contactor 0, the power input L-phase and the power input N-phase of the heating tube 32 into the plug holes 44 at the inner end and the outer end of the second conductor 46, respectively.

[0084] Step 4, connect the 220V power supply to the power L-phase input port 1 and the power N-phase input port 2 of the AC contactor 0, and press the start button 3 manually. At this time, the working power of the heating tube 32 is connected, and the heating tube 32 starts to heat. As the temperature of the heating tube 32 rises, the activation counterbore 34 on the heating plate 33 is heated, and at this time the molecular sieve starts to heat and activate.

[0085] Step 5, the temperature sensor 31 monitors the activation temperature of the molecular sieve in the activation counterbore 34. When the activation temperature is higher than the temperature threshold, the heating is automatically stopped, and when the activation temperature is lower than the temperature threshold, the molecular sieve is automatically heated again for activation. At 350℃ activation temperature, 10 -3 ~10 -4 ​Pa vacuum condition activates 8 hours, makes the molecular sieve completely remove water and gas and other substances, closes the power of AC contactor 0 and vacuum pumping system, and the activation ends.

[0086] The above is only used to illustrate the technical solutions of the present application, but not limit it. For ordinary skilled in the art, the specific technical solutions recorded in the above examples can be modified, or some technical features can be replaced equivalently, and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions protected by the present application.

Claims

1. A high-purity germanium detector molecular sieve activation device under vacuum sealing conditions, characterized by: It includes a vacuum sealing unit, an activation unit, an automatic control unit and a temperature sensor (31); The vacuum sealing unit comprises a vacuum activated container (20), and a first sealing transition structure (29) and two second sealing transition structures (30) sealingly arranged on the side wall of the vacuum activated container (20); The activation unit includes a heating tube (32), a heating plate (33) and an insulating bracket (35); The heating plate (33) is a hollow box structure, which is installed in the vacuum activation container (20) through an insulating bracket (35); a plurality of activation sinks (34) for placing molecular sieves are provided on the upper surface of the top plate of the heating plate (33); an empty slot adapted to the structure of the heating tube (32) is provided inside the heating plate (33), and the heating tube (32) is arranged in the empty slot; The automatic control unit comprises an AC contactor (0), a temperature controller (13) and a start button (3); the AC contactor (0) comprises an iron core (4) and a KM coil (5) wound on the iron core (4); The A2 terminal of the KM coil (5) is connected to the power supply N-phase input port (2) of the AC contactor (0), and the A1 terminal is connected to the output voltage L-phase port (10) of the temperature controller (13); the input voltage L-phase port (9) of the temperature controller (13) is connected to the power supply L-phase input port (1) of the AC contactor (0) via the start button (3); the input voltage N-phase port (8) of the temperature controller (13) is connected to the power supply N-phase input port (2) of the AC contactor (0); The temperature sensor (31) is mounted on the top plate of the heating plate (33) and is used to monitor the activation temperature of the molecular sieve in the activated sink hole (34). The positive signal output terminal and the negative signal output terminal of the temperature sensor (31) are connected to two inner end interfaces of the first sealing adapter structure (29), and the two outer end interfaces of the first sealing adapter structure (29) are respectively connected to the first signal input port (11) and the second signal input port (12) of the temperature controller (13); The L-phase output port (6) and the N-phase output port (7) of the AC contactor (0) are respectively connected to the outer end interfaces of the two second sealed adapter structures (30), and the inner end interfaces of the two second sealed adapter structures (30) are respectively connected to the power input L-phase and power input N-phase of the heating tube (32).

2. The high-purity germanium detector molecular sieve activation device under vacuum sealing conditions according to claim 1, characterized in that: The vacuum activated container (20) comprises a stainless steel tank body (26) with an open upper end and a flange sealing cover (21); the flange sealing cover (21) is sealedly connected to the upper end of the stainless steel tank body (26) via a hinge assembly (25); A mounting through hole is provided on the side wall of the stainless steel tank body (26), and a vacuum negative pressure gauge (23) is installed outside the mounting through hole; A vacuum interface (28) and a pressure relief valve (27) are provided on the side wall of the stainless steel tank body (26); The first sealing transition structure (29) and the two second sealing transition structures (30) are sealed and connected to the side wall of the stainless steel tank body (26).

3. The high-purity germanium detector molecular sieve activation device under vacuum sealing conditions according to claim 2, characterized in that: The first sealing transition structure (29) comprises a vacuum transition interface A, a vacuum transition interface B, two first electrical conductors (42) and a first clamp; The vacuum adapter interface A and the side wall of the stainless steel tank body (26) are an integrated structure, and two first threaded through holes are axially opened thereon; The vacuum transfer interface B comprises a first shell (41) and two first sealing blind plates (43); two second threaded through holes are axially provided on the first shell (41) at positions corresponding to the two first threaded through holes; external threads are respectively provided on the outer side walls of one end of the two first conductors (42), for being threadedly connected to the corresponding second threaded through holes and the first threaded through holes in sequence; the two first sealing blind plates (43) are respectively sleeved on the positions of the corresponding first conductors (42) connected to the first shell (41), for realizing the fixed connection between the two first conductors (42) and the first shell (41); The first clamp is arranged on the outer side wall of the first housing (41) at the connection position between the vacuum transfer interface A and the vacuum transfer interface B, and is used to realize the fixed connection between the vacuum transfer interface A and the vacuum transfer interface B; The first conductor (42) is closed in the middle and has axially opened insertion holes (44) at both ends; the insertion holes (44) at the inner ends of the two first conductors (42) serve as two inner end interfaces of the first sealing transition structure (29), and the insertion holes (44) at the outer ends serve as two outer end interfaces of the first sealing transition structure (29); The two second sealing transition structures (30) respectively include a vacuum transition interface C, a vacuum transition interface D, a second conductor (46) and a second clamp; The vacuum adapter interface C and the side wall of the stainless steel tank body (26) are an integrated structure, and a third threaded through hole is axially opened on the vacuum adapter interface C; The vacuum transfer interface D comprises a second shell (45) and a second sealing blind plate (47); a fourth threaded through hole is axially opened on the second shell (45) at a position corresponding to the third threaded through hole; an external thread is provided on an outer side wall of one end of the second conductor (46) for threaded connection with the fourth threaded through hole and the third threaded through hole in sequence; the second sealing blind plate (47) is sleeved on the second conductor (46) at a position connected to the second shell (45) for achieving a fixed connection between the second conductor (46) and the second shell (45); The second clamp is arranged on the outer side wall of the second housing (45) at the connection position between the vacuum transfer interface C and the vacuum transfer interface D, and is used to realize the fixed connection between the vacuum transfer interface C and the vacuum transfer interface D; The middle of the second conductor (46) is closed and axially provided with insertion holes (44) at both ends; the insertion hole (44) at the inner end of the second conductor (46) serves as the inner end interface of the second sealing transition structure (30), and the insertion hole (44) at the outer end serves as the outer end interface of the second sealing transition structure (30).

4. The high-purity germanium detector molecular sieve activation device under vacuum sealing conditions according to claim 3, characterized in that: The signal output positive terminal and signal output negative terminal of the temperature sensor (31), the signal first input port (11) and signal second input port (12) of the temperature controller (13), the L-phase output port (6) and N-phase output port (7) of the AC contactor (0), and the connection terminals of the wires on the power input L-phase and power input N-phase of the heating tube (32) are all configured as copper-nickel-plated banana plug structures; The jacks (44) at the inner and outer ends of the first conductor (42) and the second conductor (46) are both configured as high-conductivity oxygen-free copper jacks compatible with a banana plug structure, and are used to connect and cooperate with the corresponding banana plug structure; A groove (40) is respectively provided on one end surface of the first shell (41) facing the vacuum interface A and one end surface of the second shell (45) facing the vacuum interface C; a fluororubber ring with a bracket is respectively provided in each groove (40) for achieving a sealed connection at the corresponding interface.

5. The high-purity germanium detector molecular sieve activation device under vacuum sealing conditions according to claim 4, characterized in that: The vacuum interface (28), vacuum transfer interface A, and vacuum transfer interface C are all KF40 vacuum interfaces made of stainless steel; The vacuum transfer interface B and the vacuum transfer interface D are both KF40 vacuum interfaces made of polytetrafluoroethylene material; The insulating bracket (35) is made of polyimide insulating material; The heating tube (32) is O-shaped.

6. The high-purity germanium detector molecular sieve activation device under vacuum sealing conditions according to any one of claims 2 to 5, characterized in that: The upper end of the outer wall of the insulating bracket (35) is provided with an external thread for being threadedly connected to the bottom plate of the heating plate (33); the lower end of the insulating bracket (35) is provided with a pointed structure, and the pointed structure contacts the upper surface of the bottom of the stainless steel tank body (26), so as to support it on the bottom of the stainless steel tank body (26) and achieve a small contact area.

7. The high-purity germanium detector molecular sieve activation device under vacuum sealing conditions according to claim 1, characterized in that: The temperature sensor (31) is a Pt100 platinum resistance temperature sensor.

8. The high-purity germanium detector molecular sieve activation device under vacuum sealing conditions according to claim 3, characterized in that: The stainless steel tank body (26) and the flange sealing cover (21) are sealed via a first sealing ring (24); The first conductor (42) and the first housing (41) are sealed via a second sealing ring (48); The second conductor (46) and the second housing (45) are sealed via a third sealing ring (49).

9. The high-purity germanium detector molecular sieve activation device under vacuum sealing conditions according to claim 2, characterized in that: The stainless steel tank body (26) and the flange sealing cover (21) are both made of stainless steel; the size of the stainless steel tank body (26) is The wall thickness is 5mm, and the size of the flange sealing cover (21) is The size of the heating plate (33) is There are 13 heating plates on the top plate of the heating plate (33). activated sink (34).

10. A method for activating a high-purity germanium detector molecular sieve under vacuum sealing conditions, characterized in that: Step 1, constructing a high-purity germanium detector molecular sieve activation device under vacuum sealing conditions as described in any one of claims 1 to 9, and placing the high-purity germanium detector molecular sieve in an activation sink (34) on a heating plate (33); Step 2, connecting the vacuum interface (28) to the external vacuum pumping system, and starting the vacuum pumping system to perform high vacuum pumping; Step 3, respectively connecting the signal output positive terminal and the signal output negative terminal of the temperature sensor (31) to the two inner end interfaces of the first sealed transfer structure (29), and respectively connecting the signal first input port (11) and the signal second input port (12) of the temperature controller (13) to the two outer end interfaces of the first sealed transfer structure (29); at the same time, respectively connecting the L-phase output port (6) and the N-phase output port (7) of the AC contactor (0) to the outer end interfaces of the two second sealed transfer structures (30), and respectively connecting the inner end interfaces of the two second sealed transfer structures (30) to the power input L phase and the power input N phase of the heating tube (32); Step 4: Connect a 220V power supply to the L-phase input port (1) and the N-phase input port (2) of the AC contactor (0), and manually press the start button (3), so that the heating tube (32) starts heating, thereby heating and activating the molecular sieve in the activation sink (34); In step 5, the temperature sensor (31) monitors the activation temperature of the molecular sieve in the activation sink (34). When the activation temperature is higher than the temperature threshold, the heating is automatically stopped. When the activation temperature is lower than the temperature threshold, the molecular sieve is automatically heated again for activation until the molecular sieve activation is completed.

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