Device and method for activating molecular sieve of high-purity germanium detector under vacuum sealing condition

Abstract

The invention provides a device and a method for activating a molecular sieve of a high-purity germanium detector under a vacuum sealing condition, which are used for solving the technical problems of unstable adsorption performance and quality, poor adsorption effect and poor economical efficiency of the molecular sieve caused by low efficiency, complex operation and difficult process guarantee in the existing molecular sieve activation method. According to the molecular sieve activation device of the high-purity germanium detector under the vacuum sealing condition, the alternating current contactor, the temperature controller and the start button form an automatic control unit, and the automatic control unit is matched with the temperature sensor and the heating pipe respectively, so that the molecular sieve activation device has a temperature monitoring function; automatic stopping and automatic heating of heating activation of the molecular sieve are realized by monitoring the temperature; the device is simple in structure and convenient to control, not only has the functions of activating and vacuum storage of batch molecular sieves, can save the operation cost and improve the activation efficiency, but also has the high-vacuum high-temperature baking and degassing functions of the vacuum assembly.

Description

Technical Field

[0001] The invention relates to a molecular sieve activation device, in particular to a molecular sieve activation device and an activation method for a high-purity germanium detector under vacuum sealing conditions. Background Art

[0002] High-purity Germanium (HPGe) detectors have been widely used in many fields such as scientific research and industrial and agricultural production due to their advantages such as 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 kind of aluminosilicate compound with a cubic lattice. It has a uniform cavity-like unit cell microporous structure. The microporous structure is a grid-like porous structure formed by the windows between the cavity unit cells. Molecules with a diameter smaller than the window can pass through the window and be adsorbed on the inner surface of the unit cell. Molecular sieves have preferential adsorption capacity for polar molecules and unsaturated molecules. At liquid nitrogen temperature (77K), molecular sieves can adsorb gases 110 times their own volume, so that the vacuum chamber originally at standard atmospheric pressure can obtain a vacuum degree of 1.33Pa. Because molecular sieves have the advantages of high adsorption capacity and strong thermal stability, they are often used as low-temperature adsorbents to improve the vacuum degree of the vacuum chamber of HPGe detectors. A molecular sieve is installed between the first-stage amplifier circuit and the base flange in the vacuum chamber of the HPGe detector. This structural layout facilitates the removal and replacement of the molecular sieve. At the same time, a molecular sieve is placed in the joint of the cold finger that can be detached from the vacuum chamber of the HPGe detector to ensure and maintain the vacuum degree of the cold finger during low-temperature operation.

[0003] When using molecular sieves as low-temperature adsorbents for HPGe detectors, it should be noted that when the molecular sieves absorb a large amount of water vapor in the atmosphere, their adsorption capacity will be greatly reduced. Generally, the water content should not exceed 2%. Molecular sieves should be avoided from being exposed to the atmosphere during use, because molecular sieves can absorb more than 2% of water in the atmosphere within a few hours. When the molecular sieves absorb water and other substances to saturation, the molecular sieves will fail, destroying the vacuum degree in the vacuum chamber of the HPGe detector, directly leading to a decrease in its insulation performance. When the molecular sieve fails, it needs to be baked in a vacuum environment to discharge the water and other substances in the molecular sieve and restore the adsorption performance of the adsorption center on the surface of the molecular sieve. This is the activation of the molecular sieve.

[0004] When the vacuum chamber of the HPGe detector is opened for maintenance, the molecular sieve will be exposed to the ambient atmosphere and cause saturation failure, or after long-term use, the molecular sieve will adsorb the surface outgassing and other substances of the substances in the vacuum chamber, and its adsorption performance will decrease until saturation failure. Since the temperature of the HPGe detector during high vacuum heat treatment (60-120°C) is much lower than the temperature of molecular sieve activation (~350°C), the saturated and failed molecular sieve cannot be effectively activated, resulting in the inability to completely remove the adsorbed moisture and gas substances, which will affect the low-temperature absorption performance and further reduce the energy resolution of the HPGe detector. In addition, before packaging the internal components of the newly designed and processed HPGe detector vacuum chamber, high vacuum and high temperature baking is also required to remove surface adsorbed substances and reduce surface outgassing. Since the purity of the germanium crystal in the vacuum chamber of the HPGe detector is extremely high (99.99999999999% to 99.999999999999%), when other impurities are adsorbed on the surface of the germanium crystal, it will seriously affect the surface state of the crystal, resulting in dark current noise, causing a serious decline in the performance indicators of the HPGe detector such as energy resolution. Therefore, for the molecular sieve used as a low-temperature adsorbent for the HPGe detector, it is necessary to remove not only the adsorbed water vapor during activation, but also other adsorbed substances efficiently. In addition, the molecular sieve should not adsorb other impurities during the activation process. During the high-temperature activation process, the adsorbed water vapor and other substances need to be extracted through a high vacuum system to enable the molecular sieve to be efficiently activated and purified in high vacuum. Therefore, it is necessary to design a vacuum sealing device for the activation of high-purity germanium detector molecular sieves to achieve high-temperature and high-vacuum activation of saturated and failed molecular sieves.

[0005] Chinese patent CN 206027728 U discloses a molecular sieve activation and regeneration device, the device mainly includes a nitrogen source, a bracket and a heater. Although the technical solution can remove the residual gas and moisture in the columnar molecular sieve container through the nitrogen source, it is helpful for the activation of the molecular sieve. However, since the cylindrical heating element is wrapped in the side wall of the columnar molecular sieve container, it is impossible to ensure that each molecular sieve can be evenly heated, resulting in the dehydration performance of the molecular sieve being less than ideal. Chinese patent CN 103316631 A discloses a molecular sieve activation treatment process, which mainly includes the first heating and drying process, the second heating vacuumization, the third nitrogen filling replacement and the fourth nitrogen filling preservation process. When the molecular sieve is activated, it is installed in the activation tank, and the activation tank is inserted into the activation furnace, so it is also difficult to ensure that the molecular sieves in different parts of the activation tank are heated evenly, and only vacuumization is done in the second process during the activation process, and nitrogen needs to be flushed after the activation is completed and stored for standby. Therefore, it can be seen that the current existing molecular sieve activation treatment process has complicated and different steps, and the principle and process are basically similar to the above-mentioned public documents. It is mainly aimed at the application of molecular sieves in the industrial field. It is usually heated to the activation temperature by high-temperature gas purging, but the gas specific heat capacity is small and the heating efficiency is low. And when the existing activation device heats the molecular sieve, the molecular sieve is often heated unevenly, and the molecular sieve cannot be fully dried, resulting in the dehumidification efficiency and effect of the molecular sieve being not excellent enough, so that the effect of the molecular sieve is limited when it is used next time. In summary, the existing molecular sieve activation method is inefficient, complicated to operate, and the process is difficult to guarantee, resulting in unstable adsorption performance and quality of the molecular sieve, poor adsorption effect and poor economy. Summary of the invention

[0006] The purpose of the present invention is to solve the technical problems of low efficiency, complex operation and difficult process guarantee in the existing molecular sieve activation methods, which lead 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 object, the technical solution provided by the present invention is as follows:

[0008] A high-purity germanium detector molecular sieve activation device under vacuum sealing conditions, which is special in that it includes a vacuum sealing unit, an activation unit, an automatic control unit and a temperature sensor;

[0009] The vacuum sealing unit comprises a vacuum activated container, and a first sealing transition structure and two second sealing transition structures which are sealingly arranged on the side wall of the vacuum activated container;

[0010] The activation unit comprises a heating tube, a heating plate and an insulating bracket;

[0011] The heating plate is a hollow box structure, which is installed in a vacuum activation container through an insulating bracket; a plurality of activation sinks for placing molecular sieves are arranged on the upper surface of the top plate of the heating plate; an empty slot adapted to the heating tube structure is arranged inside the heating plate, and the heating tube is arranged in the empty slot;

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

[0013] The A2 terminal of the KM coil is connected to the power supply N-phase input port of the AC contactor, and the A1 terminal is connected to the output voltage L-phase port of the temperature controller; the input voltage L-phase port of the temperature controller is connected to the power supply L-phase input port of the AC contactor through a start button; the input voltage N-phase port of the temperature controller is connected to 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 is used to monitor the activation temperature of the molecular sieve in the activated sink hole. The signal output positive end and the signal output negative end are connected to the two inner end interfaces of the first sealing adapter structure, and the two outer end interfaces of the first sealing adapter structure are respectively connected to the first signal input port and the second signal 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 to the outer end interfaces of the two second sealed adapter structures, and the inner end interfaces of the two second sealed adapter structures are respectively connected to the power input L-phase and power input N-phase of the heating tube.

[0016] Furthermore, the vacuum activated container comprises a stainless steel tank body with an upper opening and a flange sealing cover; the flange sealing cover is sealed and connected to the upper end of the stainless steel tank body through a hinge assembly;

[0017] A mounting through hole is provided on the side wall of the stainless steel tank body, and the vacuum negative pressure gauge is installed outside the mounting through hole;

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

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

[0020] Furthermore, the first sealing transition structure includes a vacuum transition interface A, a vacuum transition interface B, two first conductors 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 has two first threaded through holes axially formed thereon;

[0022] The vacuum transfer interface B comprises a first shell and two first sealing blind plates; two second threaded through holes are axially provided at positions corresponding to the two first threaded through holes on the first shell; external threads are respectively provided on the outer side walls of one end of the two first conductors, which are used to be threadedly connected with the corresponding second threaded through holes and the first threaded through holes in sequence; the two first sealing blind plates are respectively sleeved on the positions of the corresponding first conductors connected to the first shell, which are used to realize the fixed connection between the two first conductors and the first shell;

[0023] The first clamp is arranged on the outer side wall of the first shell connecting position of 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;

[0024] The first conductor is closed in the middle and has axially opened holes at both ends; the holes at the inner ends of the two first conductors serve as two inner end interfaces of the first sealed adapter structure, and the holes at the outer ends serve as two outer end interfaces of the first sealed adapter structure;

[0025] The two second sealing transition structures respectively include a vacuum transition interface C, a vacuum transition interface D, a second conductor and a second clamp;

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

[0027] The vacuum transfer interface D comprises a second shell and a second sealing blind plate; a fourth threaded through hole is axially opened at a position corresponding to the third threaded through hole on the second shell; an external thread is arranged on an outer side wall of one end of the second conductor, which is threadedly connected with the fourth threaded through hole and the third threaded through hole in sequence; the second sealing blind plate is sleeved on the second conductor at a position connected with the second shell, which is used to realize the fixed connection between the second conductor and the second shell;

[0028] The second clamp is arranged on the outer side wall of the second housing connection position of 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;

[0029] The middle of the second conductor is closed and both ends are axially provided with insertion holes; the insertion hole at the inner end of the second conductor serves as the inner end interface of the second sealed transition structure, and the insertion hole at the outer end serves as the outer end interface of the second sealed transition structure.

[0030] Furthermore, the signal output positive terminal and signal output negative terminal of the temperature sensor, the signal first input port and signal second input port of the temperature controller, the L-phase output port and N-phase output port of the AC contactor, and the wiring terminals of the wires on the power input L-phase and power input N-phase of the heating tube are all set to a banana plug structure of copper-nickel-plated material;

[0031] The jacks at the inner and outer ends of the first and second conductors are both configured as high-conductivity oxygen-free copper jacks that match the banana plug structure, and are used to connect and cooperate with the corresponding banana plug structure;

[0032] A groove is respectively formed on one end surface of the first shell facing the vacuum interface A and one end surface of the second shell facing the vacuum interface C; a fluororubber ring with a bracket is respectively arranged in each groove to achieve a sealed connection at the corresponding interface.

[0033] Furthermore, the vacuum interface, vacuum transfer interface A, and vacuum transfer interface C are all KF40 vacuum interfaces made of stainless steel;

[0034] The vacuum transfer interface B and the vacuum transfer interface D are both KF40 vacuum interfaces made of polytetrafluoroethylene material;

[0035] The insulating bracket is made of polyimide insulating material;

[0036] The heating tube is O-shaped.

[0037] Furthermore, an external thread is provided at the upper end of the outer wall of the insulating bracket for threaded connection with the bottom plate of the heating plate; the lower end of the insulating bracket is provided with a pointed structure, and the pointed structure contacts the bottom upper surface of the stainless steel tank body, so as to support it at the bottom of the stainless steel tank body and achieve a small contact area.

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

[0039] Furthermore, 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] Furthermore, 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 The wall thickness is 5mm and the size of the flange sealing cover is

[0043] The size of the heating plate is There are 13 heating plates on the top plate. Activated sink hole.

[0044] In addition, the present invention also provides an activation method for the high-purity germanium detector molecular sieve activation device under vacuum sealing conditions, which is special in that:

[0045] Step 1, placing a high-purity germanium detector molecular sieve in an activated sink hole on a 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, respectively connect the signal output positive terminal and the signal output negative terminal of the temperature sensor to the two inner end interfaces of the first sealed adapter structure, and respectively connect the signal first input port and the signal second input port of the temperature controller to the two outer end interfaces of the first sealed adapter structure; at the same time, respectively 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, and respectively connect the inner end interfaces of the two second sealed adapter structures to the power input L phase and the power input N phase of the heating tube;

[0048] Step 4, connect 220V power to the L-phase input port and the N-phase input port of the AC contactor, and manually press the start button, the heating tube starts to heat, and then the molecular sieve in the activated sink hole starts to heat and activate;

[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] Compared with the prior art, the present invention has the following beneficial effects:

[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 respectively 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 is convenient to control. It not only has the activation and vacuum preservation functions of batch molecular sieves, can save operating costs and improve activation efficiency, but also has the high-vacuum and high-temperature baking and degassing function of vacuum components.

[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 makes a special structural design 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 of 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 It is a structural schematic diagram of an embodiment of a molecular sieve activation device for a high-purity germanium detector under vacuum sealing conditions of the present invention;

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

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

[0057] Figure 4 Schematic diagram of the structure of the second sealing transition structure in an embodiment of the present invention;

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

[0059] The specific reference numerals are as follows:

[0060] 0-AC contactor; 1-power L-phase input port; 2-power 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 first input port; 12-signal second input port; 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 - insertion hole; 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 invention more clear, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0065] like Figure 1 , Figure 2 As shown, a high-purity germanium detector molecular sieve activation device under vacuum sealing conditions is suitable for activating molecular sieves in the germanium crystal vacuum chamber and cold finger joint of the high-purity germanium detector, which includes a vacuum sealing unit, an activation unit, an automatic control unit and a temperature sensor 31.

[0066] The vacuum sealing unit is used to achieve high vacuum sealing and molecular sieve vacuum preservation during the molecular sieve activation process. The vacuum sealing unit includes a vacuum activation container 20, a first sealing transition structure 29 and two second sealing transition 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 sealed to the upper end of the stainless steel tank body 26 by a hinge assembly 25, which is convenient for inspecting and repairing the components in the stainless steel tank body 26. The flange sealing cover 21 is a structure without fixing bolts, and the vacuum seal between the stainless steel tank body 26 and the flange sealing cover 21 is achieved by using the internal negative pressure and the first sealing ring 24. The stainless steel tank body 26 and the flange sealing cover 21 are both made of stainless steel. In this embodiment, 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

[0067] The side wall of the stainless steel tank 26 is provided with a mounting hole, and the vacuum negative pressure gauge 23 is installed outside the mounting hole to monitor the negative pressure value inside the vacuum activation container 20. At the same time, the side wall of the stainless steel tank 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 to perform high vacuum pumping during the entire activation process of the molecular sieve, and 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 baffle valve, which is used to relieve the internal pressure of the vacuum activation container 20.

[0068] The activation unit is used to realize the high temperature activation function of the molecular sieve, which includes a heating plate 33, a heating tube 32 and an insulating bracket 35. The heating plate 33 is a hollow box structure, which is surrounded by a top plate, a bottom plate and side plates around it, and is connected by countersunk screws. The insulating bracket 35 is placed on the inner bottom plate of the vacuum activation container 20, and the heating plate 33 is installed on the upper end of the insulating bracket 35. Since polyimide has the performance of high temperature resistance of 400°C, tensile strength of more than 100MPa, good dielectric properties, small thermal expansion coefficient, and low outgassing under extremely high vacuum, it meets the high temperature and high vacuum working environment during the activation of the molecular sieve, so the insulating bracket 35 preferably uses polyimide for insulating support. Specifically, the upper end of the outer wall of the insulating bracket 35 is provided with an external thread for threaded connection with the bottom plate of the heating plate 33, and its lower end is in contact with the bottom upper surface of the stainless steel tank body 26, so as to support it at the bottom of the stainless steel tank body 26. Preferably, the lower end of the insulating bracket 35 is configured as a pointed structure, which can effectively reduce the contact area between the insulating bracket 35 and the bottom of the stainless steel tank 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 Φ18mm×20mm, each of which is used to place the molecular sieve, and the molecular sieve is activated in batches through the thirteen activation countersunk holes 34. At the same time, the interior of the heating plate 33 is provided with an empty slot adapted to the structure of the heating tube 32 in the vertical direction, and the heating tube 32 is placed in the empty slot to transfer the heat of the heating tube 32 to the heating plate 33. In this embodiment, the heating tube 32 is preferably set to O-type, and accordingly, the structure of the empty slot is also O-type.

[0070] The automatic control unit is used to realize the automatic opening and closing function of the molecular sieve high temperature activation. It is installed in a control box, which can make the vacuum sealing unit compact and easy to connect. 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 also provided with a power supply L-phase input port 1, a power supply N-phase input port 2, an L-phase output port 6 and an N-phase output port 7. A temperature threshold is set in the temperature controller 13, and 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 are provided on the temperature controller 13.

[0071] 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 through 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.

[0072] The temperature sensor 31 is installed on the top plate of the heating plate 33 and is used to monitor the activation temperature of the molecular sieve in the activation sink 34. The signal output positive end and the signal output negative end of the temperature sensor 31 are respectively connected to the 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 signal first input port 11 and the signal second input port 12 of the temperature controller 13. Among them, the temperature controller 13 is used to monitor the temperature of the molecular sieve during the activation process through the signal input by the temperature sensor 31, and control the contact of the AC contactor 0 to open and close the circuit according to the monitored temperature. In this embodiment, the temperature sensor 31 adopts a Pt100 platinum resistance temperature sensor, and other temperature sensors can also be used in other embodiments of the present invention. The input of the power supply L phase input port 1 and the power supply N phase input port 2 is a 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 to 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 to the power input L-phase and power input N-phase of the heating tube 32, which are used to open and close the circuit through the contacts of the AC contactor 0 to realize the connection and disconnection of the working power of the O-type heating tube 32.

[0074] The working principle of the automatic control unit is as follows: when the power supply L phase input port 1 and the power supply N phase input port 2 are kept at 220V, the start button 3 is pressed, the output voltage L phase port 10 of the temperature controller 13 is connected, the KM coil 5 of the AC contactor 0 is energized, the iron core 4 generates electromagnetic attraction, the suction contact is closed, and the power is turned on, the output voltage of the L phase output port 6 and the N phase output port 7 is connected, and the working power is provided to the heating tube 32. The heating tube 32 heats and transfers the heat to the activation sink hole 34 in the heating plate 33, and the molecular sieve placed in the activation sink hole 34 begins to be activated at high temperature.

[0075] The temperature sensor 31 monitors the temperature in the activation sink hole 34. When the temperature monitored by the temperature sensor 31 is higher than the threshold value, the output voltage L-phase port 10 of the temperature controller 13 is 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 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 connected again, the contacts of the AC contactor 0 are closed, the working power of the heating tube 32 is connected again, and the molecular sieve placed in the activation sink hole 34 is activated again at high temperature.

[0076] At the same time, the present invention has specially designed the first sealing transition structure 29 and the second sealing transition structure 30. Figure 3 As shown, the first sealing transition structure 29 includes a vacuum transition interface A, a vacuum transition interface B, two first conductors 42 and a first clamp; the vacuum transition interface A is arranged on the stainless steel tank body 26, and is an integrated structure with the side wall of the stainless steel tank body 26, and two first threaded through holes are axially opened thereon. The vacuum transition interface B includes a first shell 41 and two first sealing blind plates 43; two second threaded through holes are axially opened at positions corresponding to the two first threaded through holes on the first shell 41, and external threads are respectively arranged on the outer side walls at one end of the two first conductors 42, which are used to be threadedly connected with 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, which are used to realize the fixed connection between the two first conductors 42 and the first shell 41; at the same time, the sealing between the first conductor 42 and the first shell 41 is realized by the second sealing ring 48. The first clamp is arranged on the outer side wall of the connecting position of the first shell 41 of 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; a groove 40 is provided on the end face of the first shell 41 facing the vacuum interface A, and a fluororubber ring with a bracket is provided in the groove 40, which is used to realize the sealing at the interface between the vacuum transfer interface A and the first shell 41.

[0077] The first conductor 42 is closed in the middle and has axially opened sockets 44 at both ends; the sockets 44 at the inner ends of the two first conductors 42 serve as the two inner end interfaces of the first sealed adapter structure 29, and the sockets 44 at the outer ends serve as the two outer end interfaces of the first sealed adapter structure 29. The wire connection terminals on the positive signal output terminal and the negative signal output terminal of the temperature sensor 31, the first signal input port 11 and the second signal input port 12 of the temperature controller 13 are all banana plug structures made of copper-plated nickel. The sockets 44 at the inner end and the sockets 44 at the outer end of the first conductor 42 are both high-conductivity oxygen-free copper sockets that match the banana plug structure. The banana plug structure made of copper-plated nickel and the high-conductivity oxygen-free copper socket cooperate to realize the conduction of the connection line. This connection is light and fast, and has excellent conduction performance.

[0078] Since the voltage output by the L-phase output port 6 and the N-phase output port 7 of the AC contactor 0 is 220V high voltage, the sealing transition structures corresponding to the L-phase output port 6 and the N-phase output port 7 are separately provided, that is, two second sealing transition structures 30 are provided, which can effectively avoid short circuit between the two line contacts. Figure 4 As shown, the structures of the two second sealing transition structures 30 are similar to those of the first sealing transition structure 29, and both include a vacuum transition interface C, a vacuum transition interface D, a second conductor 46, and a second clamp. The vacuum transition interface C is an integrated structure with the side wall of the stainless steel tank body 26, and a third threaded through hole is axially opened thereon. The vacuum transition interface D includes a second shell 45 and a second sealing blind plate 47, and 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 the outer wall of one end of the second conductor 46, which is used to be threadedly connected 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, which is used to realize the fixed connection between the second conductor 46 and the second shell 45; at the same time, the sealing between the second conductor 46 and the second shell 45 is realized by the third sealing ring 49. The second clamp is arranged on the outer side wall of the second shell 45 connecting 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; similarly, a groove 40 is provided on the end face of one end of the second shell 45 facing the vacuum interface C, and a fluororubber ring with a bracket is provided in the groove 40, which is used to realize the sealing at the interface between the vacuum transfer interface C and the second shell 45.

[0079] The middle of the second conductor 46 is closed and the two ends are axially provided with a socket 44. The socket 44 at the inner end of the second conductor 46 serves as the inner end interface of the second sealed adapter structure 30, and the socket 44 at the outer end serves as 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 wires on the power input L-phase and the power input N-phase of the heating tube 32 are all copper-nickel-plated banana plug structures, and the sockets 44 at the inner ends and the sockets 44 at the outer ends of the two second conductors 46 are high-conductivity oxygen-free copper sockets that match the outer diameter of the banana plug structure, which are used to cooperate to achieve the conduction of the connection line. Preferably, the vacuum interface 28, the vacuum adapter interface A and the vacuum adapter interface C of this embodiment are all stainless steel KF40 vacuum interfaces, and the vacuum adapter interface B and the vacuum adapter interface D are all polytetrafluoroethylene KF40 vacuum interfaces.

[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: Figure 5 The high purity germanium detector molecular sieve shown is placed in the activation sink hole 34 on the heating plate 33, and the flange sealing cover 21 is closed.

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

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

[0084] Step 4, connect 220V power to the power L-phase input port 1 and the power N-phase input port 2 of the AC contactor 0, and manually press the start button 3. 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 increases, the activation sink 34 on the heating plate 33 is heated, and 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 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. -3 ~10 -4Pa vacuum conditions for 8 hours to completely remove moisture, gas and other substances from the molecular sieve, turn off the power of the AC contactor 0 and the vacuum pumping system, and the activation is completed.

[0086] The above description is only used to illustrate the technical solution of the present invention rather than to limit it. For ordinary professional and technical personnel in the field, the specific technical solution recorded in the above embodiment can be modified, or some of the technical features therein can be replaced by equivalents, and these modifications or replacements do not make the essence of the corresponding technical solution deviate from the scope of the technical solution protected by the present invention.

Claims

1. A high-purity germanium detector molecular sieve activation device under vacuum sealing conditions, characterized in that: 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) which are sealingly arranged on the side wall of the vacuum activated container (20); The activation unit comprises 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 arranged on the upper surface of the top plate of the heating plate (33); an empty groove matching the structure of the heating tube (32) is arranged inside the heating plate (33), and the heating tube (32) is arranged in the empty groove; 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 a 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 installed on the top plate of the heating plate (33) and is used to monitor the activation temperature of the molecular sieve in the activation sink (34). The signal output positive end and the signal output negative end 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 opening at the 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 the 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 sealingly 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 provided 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 at positions corresponding to the two first threaded through holes on the first shell (41); external threads are respectively provided on the outer side walls of one end of the two first conductors (42) for threaded connection with 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 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 shell (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 comprise 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 thereon; 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 at a position corresponding to the third threaded through hole on the second shell (45); an outer wall at one end of the second conductor (46) is provided with an external thread, which is used to be threadedly connected 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), so as to realize the 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 both ends are axially provided with insertion holes (44); 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 arranged as banana plug structures made of copper-plated nickel material; The sockets (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 sockets that match the banana plug structure, and are used to achieve connection and matching with the corresponding banana plug structure; A groove (40) is respectively formed 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 arranged in each groove (40) to achieve 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 threaded connection with 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 at 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 shell (41) are sealed via a second sealing ring (48); The second conductor (46) and the second shell (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 5 mm, and the size of the flange sealing cover (21) is The size of the heating plate (33) is The top plate of the heating plate (33) is provided with 13 The activated sink hole (34) is provided.

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 an 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 adapter 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 adapter 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 adapter structures (30), and respectively connecting the inner end interfaces of the two second sealed adapter structures (30) to the power input L phase and the power input N phase of the heating tube (32); Step 4, connect 220V power to the power L-phase input port (1) and the power N-phase input port (2) of the AC contactor (0), and manually press the start button (3), the heating tube (32) starts heating, and then the molecular sieve in the activation sink (34) starts heating and activation; Step 5, the temperature sensor (31) monitors the activation temperature of the molecular sieve in the activation sink (34), and automatically stops heating when the activation temperature is higher than the temperature threshold, and automatically heats the molecular sieve again for activation when the activation temperature is lower than the temperature threshold until the molecular sieve activation is completed.

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