WO2022148034A1 - Ceramic transfer tube and fabrication method therefor - Google Patents

Ceramic transfer tube and fabrication method therefor Download PDF

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Publication number
WO2022148034A1
WO2022148034A1 PCT/CN2021/115971 CN2021115971W WO2022148034A1 WO 2022148034 A1 WO2022148034 A1 WO 2022148034A1 CN 2021115971 W CN2021115971 W CN 2021115971W WO 2022148034 A1 WO2022148034 A1 WO 2022148034A1
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ceramic
metal electrode
annular
sheet
sheets
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PCT/CN2021/115971
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French (fr)
Chinese (zh)
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黄翌敏
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上海奕瑞光电子科技股份有限公司
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Publication of WO2022148034A1 publication Critical patent/WO2022148034A1/en

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/06Electron- or ion-optical arrangements
    • H01J49/062Ion guides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02Manufacture of electrodes or electrode systems
    • H01J9/14Manufacture of electrodes or electrode systems of non-emitting electrodes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • the present application relates to the technical field of trace detection, and in particular, to a ceramic migration tube and a manufacturing method thereof.
  • Ion mobility spectrometer has the advantages of sensitivity, rapidity, low power consumption and portability.
  • the use of ion migration detection technology has greatly strengthened the monitoring of personnel and luggage at important borders such as border defense, customs, and civil aviation, and effectively combated the implementation of smuggling, drug trafficking and terrorist attacks.
  • the migration tube is the core component of the ion mobility spectrometer, and it is also the key factor determining the separation and detection of the mobility spectrometer.
  • the migration tube of the existing commercial ion mobility spectrometer is mainly made of insulating materials such as polyimide/polytetrafluoro/peak and metal electrodes by crimping with nuts, springs and O-rings.
  • the migration tube of the existing commercial ion mobility spectrometer is difficult to assemble and seal, time-consuming and laborious, and has a high manufacturing cost, which is not conducive to the mass production of the ion mobility spectrometer and the improvement of system stability.
  • the temperature of the migration tube needs to be set at a higher working temperature.
  • it is polyimide, polytetrafluoroethylene or peak, it is difficult to work at a working temperature of more than 200 °C, and this type of migration tube will produce trace releases at high temperatures, and multiple thermal shocks will also affect the migration tube. The tightness will affect the normal use of the ion mobility spectrometer.
  • the present application provides a ceramic transfer tube and a manufacturing method thereof, so as to solve the problems of difficult assembly and sealing of the existing transfer tube, time-consuming and labor-intensive, and high manufacturing cost.
  • a ceramic migration tube includes:
  • the ionization chamber is arranged at one end of the migration chamber
  • the Faraday cup assembly is disposed at the other end of the migration chamber
  • an ion gate assembly disposed between the ionization chamber and the migration chamber;
  • the migration chamber includes a plurality of annular insulating ceramic sheets and a plurality of annular metal electrode sheets, the annular insulating ceramic sheets and the annular metal electrode sheets are alternately arranged in sequence, and the adjacent annular insulating ceramic sheets and the The annular metal electrode sheet is sealed and welded.
  • the annular insulating ceramic sheet and the annular metal electrode sheet are fixed by soldering, and the expansion coefficient of the annular metal electrode sheet is equal to or close to the expansion coefficient of the annular insulating ceramic sheet.
  • the annular insulating ceramic sheet is made of 95 porcelain or 99 porcelain, and the annular insulating ceramic sheet has a thickness of 1 mm-3 mm; and/or,
  • the annular metal electrode sheet adopts Kovar alloy, the thickness of the annular metal electrode sheet is 1mm-3mm, and/or,
  • the solder is silver-copper alloy.
  • the surface of the annular insulating ceramic sheet is metallized and treated with hydrogen burning, and the surface of the annular metal electrode sheet is cleaned and nickel-plated and treated with hydrogen burning.
  • the ionization chamber includes a source seat, a C-shaped shrapnel, and a sheet-shaped ionization source, the source seat is provided with a hollow hole therethrough, and the C-shaped shrapnel is fixed in the hollow hole with an interference fit, and the The flake ionization source is deposited on the inner wall of the C-shaped shrapnel by sputtering or evaporation;
  • a limiting boss is protrudingly arranged on the inner wall of the hollow hole for axially blocking the C-shaped shrapnel;
  • a clamping groove is provided on the radial side of the hollow hole for clamping, installing or dismounting the C-shaped elastic piece.
  • the ion gate assembly includes a first ion gate grid, a ceramic spacer, and a second ion gate; the ceramic spacer is arranged between the first ion gate and the second ion gate is used to separate the first ion gate and the second ion gate by a set distance; the ceramic spacer is sealed and welded with the first ion gate and the second ion gate.
  • the Faraday cup assembly includes a Faraday cup and a ceramic shielding cover sleeved on the Faraday cup; the surface of the Faraday cup is polished and plated with gold to reduce detector noise; the ceramic shielding cover has a metal outer ring After welding, it is equipotential with the suppression grid to shield the interference of external signals to the Faraday cup signal; the Faraday cup is sealed and welded with the ceramic shielding cover through a connecting rod.
  • a method for manufacturing a ceramic transfer tube includes:
  • a ceramic migration tube preform to be welded includes a plurality of annular insulating ceramic sheets and a plurality of annular metal electrode sheets, the annular insulating ceramic sheets and the annular metal electrode sheets are alternately arranged in sequence, Solder is arranged between the adjacent annular insulating ceramic sheet and the annular metal electrode sheet;
  • the ceramic migration tube preform to be welded is placed in a hydrogen brazing furnace, and the hydrogen brazing furnace is heated to a first preset temperature at a first preset heating rate under a hydrogen protective atmosphere, and the first preset temperature is maintained. setting a time period, wherein the first preset temperature is less than the melting point of the solder;
  • the hydrogen brazing furnace is heated to a second preset temperature at a second preset heating rate, and maintained for a second preset time period, wherein the second preset temperature is greater than or equal to the melting point of the solder, and the first preset temperature is greater than or equal to the melting point of the solder. 2.
  • the preset heating rate is less than the first preset heating rate;
  • the temperature of the hydrogen brazing furnace is lowered to a fourth preset temperature, and the hydrogen supply in the hydrogen brazing furnace is stopped.
  • the surface of the annular insulating ceramic sheet in the preform of the ceramic migration tube to be welded is metallized and hydrogen-fired, and the surface of the annular metal electrode sheet in the preform of the ceramic migration tube to be welded is cleaned and plated.
  • Nickel and hydrogen-burning treatment, the solder uses a silver-copper alloy.
  • a mounting tool is also provided, and the mounting tool coaxially fixes the plurality of annular insulating ceramic sheets and the plurality of annular metal electrode sheets in the ceramic migration tube preform to be welded.
  • FIG. 1 is a cross-sectional view of a ceramic migration tube provided by an embodiment of the present application.
  • FIG. 2 is a schematic structural diagram of the ionization chamber in FIG. 1 .
  • FIG. 3 is an exploded schematic view of the ion gate assembly in FIG. 1 .
  • FIG. 4 is a schematic structural diagram of the annular insulating ceramic sheet in FIG. 1 .
  • FIG. 5 is a schematic structural diagram of the annular metal electrode sheet in FIG. 1 .
  • FIG. 6 is a schematic structural diagram of the suppression grid and the Faraday cup assembly in FIG. 1 .
  • an embodiment of the present application provides a ceramic migration tube.
  • the ceramic migration tube includes a migration chamber 3 , an ionization chamber 1 , a Faraday cup assembly 5 , an ion gate assembly 2 and a suppression grid 4 .
  • the migration chamber 3 is used to provide a uniform weak drift electric field and an electrically neutral reverse flow field so that the mobility and different ion groups are separated in the region of the migration chamber 3 .
  • the ionization chamber 1 is arranged at one end of the migration chamber 3, and the ionization chamber 1 is used for providing ionization energy and ionization space for ionizing sample molecules or other molecules.
  • the ion gate assembly 2 is arranged between the ionization chamber 1 and the migration chamber 3, and the ion gate assembly 2 is used to provide an acceleration electric field/cut-off electric field of the ions and a migration clock signal.
  • the Faraday cup assembly 5 is disposed at the other end of the migration chamber 3, and the Faraday cup assembly 5 is used to detect ions and generate ion signals.
  • the ion groups separated by the migration chamber 3 reach the Faraday cup assembly successively to generate ion signals.
  • the suppression grid 4 is arranged between the migration chamber 3 and the Faraday cup assembly 5, and the suppression grid 4 is used to shield the interference of the ion gate pulse voltage to the signal of the Faraday cup assembly.
  • the migration chamber 3 includes a plurality of annular insulating ceramic sheets 31 and a plurality of annular metal electrode sheets 32 .
  • the annular insulating ceramic sheets 31 and the annular metal electrode sheets 32 are arranged alternately in sequence.
  • the adjacent annular insulating ceramic sheets 31 are sealed and welded to the annular metal electrode sheet 32 .
  • a plurality of annular insulating ceramic sheets 31 are arranged at intervals in sequence, and an annular metal electrode sheet 32 is disposed between every two annular insulating ceramic sheets 31 , and the annular metal electrode sheet 32 is adjacent to two annular insulating ceramic sheets 31 . Seal welded together.
  • the annular insulating ceramic sheets 31 and the annular metal electrode sheets 32 in the migration chamber 3 are arranged alternately in turn, and the adjacent annular insulating ceramic sheets 31 and the annular metal electrode sheet 32 are sealed and welded, which is convenient for installation and low in manufacturing cost; good sealing performance and reliable connection Firm, high mechanical strength, strong shock resistance, improve system stability.
  • the annular insulating ceramic sheet 31 in the migration chamber 3 has a high thermal conductivity, which can shorten the cold start time of the machine.
  • the sealing and welding structure between the adjacent annular insulating ceramic sheets 31 and the annular metal electrode sheet 32 can be specifically set as required.
  • the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32 can be fixed by soldering.
  • the expansion coefficient of the annular metal electrode sheet 32 may be equal to or close to the expansion coefficient of the annular insulating ceramic sheet 31 .
  • Solder can be made of high melting point solder, which eliminates the use of non-heat-resistant materials and high-temperature trace volatile materials. Therefore, the migration tube can work at a temperature of 250 ° C and above, which can more effectively deal with the detection of high-boiling prohibited items such as drugs and explosives. , and can improve the cleaning speed of the system.
  • the materials and thicknesses of the annular insulating ceramic sheet 31 , the annular metal electrode sheet 32 and the solder should be selected in consideration of their weldability and welding stability.
  • the annular insulating ceramic sheet 31 adopts 95 porcelain or 99 porcelain.
  • the annular insulating ceramic sheet 31 may have a thickness of 1mm-3mm.
  • the annular metal electrode sheet 32 can be made of Kovar alloy.
  • the coefficient of expansion of the Kovar alloy is close to that of the annular insulating ceramic sheet 31 .
  • the thickness of Kovar alloy can be set to 1mm-3mm.
  • the annular metal electrode sheet 32 can be made of 4J33 Kovar alloy.
  • the solder can be silver-copper alloy.
  • the high melting point of copper-silver alloy allows the migration tube to work at a higher temperature, which can more effectively deal with the detection of high-boiling prohibited items such as drugs and explosives, and can improve the cleaning speed of the system.
  • a 72:8 silver-copper alloy was used as the solder, the ratio of silver to copper was 72:8, the solidus was 779°C, and the melting point was 810°C.
  • the ionization chamber 13 includes an ionization source and a source base 11 .
  • the source seat 11 is used for installing and fixing the ionization source 13 , and its specific structure can be set according to the specific structure of the ionization source 13 .
  • the ionization source 13 can use radioactive sources such as 63Ni, 3H, or non-radioactive sources such as UV, DBD (Dielectric Barrier Discharge) and corona discharge ionization sources.
  • the ionization chamber 1 may include a source seat 11 , a C-shaped elastic sheet 12 and a sheet-shaped ionization source 13 .
  • the source seat 11 is an annular structure, and a hollow hole 111 is formed therethrough.
  • the C-shaped elastic piece 12 has elasticity, and can be elastically deformed when it is stressed.
  • the C-shaped elastic piece 12 is fixed in the hollow hole 111 by interference fit.
  • the C-shaped elastic piece 12 can be elastically deformed toward the inner side of the radial direction thereof, and abuts against the inner wall of the hollow hole 111 of the source seat 11 .
  • the sheet-shaped ionization source 13 can be deposited on the inner wall of the C-shaped elastic sheet 12 by sputtering, vapor deposition or other methods.
  • a limiting boss 112 can be protruded from the inner wall of the hollow hole 111 for axially topping off the C-shaped elastic piece 12 .
  • the limiting boss 112 can block the C-shaped shrapnel 12 to prevent the C-shaped shrapnel 12 from continuing to be inserted and prompt the C-shaped shrapnel 12 and the ionization source 13 to be installed In-place restrictions and prompts for radioactive sources to be installed in place.
  • a clamping groove 113 may be provided on the radial side of the hollow hole 111 , and the clamping groove 113 communicates with the hollow hole 111 and can be used for clamping, installing or removing the C-shaped elastic piece 12 .
  • the sheet-shaped ionization source 13 may use a 63Ni source.
  • the C-shaped elastic pieces 12 are correspondingly arranged as C-shaped nickel-based elastic pieces.
  • the sheet-shaped ionization source 13 of the 63Ni source can be evaporated on the inner wall of the C-shaped nickel-based elastic sheet.
  • the ion gate assembly 2 may include a first ion gate grid 21 , a ceramic spacer 22 and a second ion gate grid 23 .
  • the ceramic spacer 22 is disposed between the first ion gate grid 21 and the second ion gate grid 23 , and is used to space the first ion gate grid 21 and the second ion gate grid 23 by a predetermined distance.
  • the ceramic spacer 22 is sealed and welded with the first ion gate grid 21 and the second ion gate grid 23, which can prevent the molten solder from spattering/overflowing and reducing the insulation between the ion gates. More preferably, the ceramic spacer 22 is not more than 0.7 mm for isolating the first ion gate 21 and the second ion gate 23 . Correspondingly, the distance between the first ion gate grid 21 and the second ion gate grid 23 is not more than 0.7 mm.
  • the Faraday cup assembly 5 may include a Faraday cup 51 and a ceramic shield 52 .
  • the Faraday cup 51 is sealed and welded to the ceramic shield 52 through a connecting rod.
  • the ceramic shield 52 can be fitted over the connecting rod of the Faraday cup 51 .
  • the Faraday cup 51 is polished and gold plated to reduce detector noise.
  • the outer ring of the ceramic shielding cover 52 is metallized, and after welding, it is equipotential with the suppression grid 4, which is used to shield the interference of the external signal to the signal of the Faraday cup 51.
  • the Faraday cup 51 is hermetically welded to the ceramic shield 52 .
  • the Faraday cup 51 can be sealed with the shielding cover by nesting the metallized annular ceramic shielding cover 52 on the inner and outer rings on the connecting rod connecting the Faraday cup 51, and sealing with double-layer casing.
  • the specific structure of the suppression gate can be set as required, as long as it can shield the interference of the pulse voltage of the ion gate to the signal of the Faraday cup 51 .
  • the suppression grid 4 can be configured as a sheet-like grid structure, and the sheet-like grid structure can be specifically configured as a hexagon, a circle, or the like.
  • the present application also provides a method for manufacturing a ceramic transfer tube.
  • the manufacturing method of the ceramic migration tube includes:
  • the ceramic migration tube preform to be welded includes a plurality of annular insulating ceramic sheets 31 and a plurality of annular metal electrode sheets 32 . Solder is provided between the electrode pads 32 .
  • the ceramic migration tube preform to be welded is placed in a hydrogen brazing furnace, and the hydrogen brazing furnace is heated to a first preset temperature at a first preset heating rate under a hydrogen protective atmosphere, and maintained for a first preset time. section to ensure that the weldment temperature is uniform.
  • the first preset temperature is less than the melting point of the solder.
  • the hydrogen brazing furnace is heated to a second preset temperature at a second preset heating rate, and maintained for a second preset time period to ensure that the solder of each welding seam is fully melted and the welding interface is well infiltrated.
  • the second preset temperature is greater than or equal to the melting point of the solder, and the second preset heating rate is less than the first preset heating rate;
  • the hydrogen brazing furnace is cooled to a third preset temperature at a third preset cooling rate to slowly release the sealing stress of the welding seam between the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32 to prevent the ceramic from bursting.
  • the temperature of the hydrogen brazing furnace is lowered to the fourth preset temperature, and the hydrogen supply in the hydrogen brazing furnace is stopped.
  • the annular insulating ceramic sheets 31 and the annular metal electrode sheets 32 in the migration chamber 3 are alternately arranged in sequence, and the adjacent annular insulating ceramic sheets 31 and the annular metal electrode sheet 32 are sealed and welded by solder, which is integrally formed and easy to install.
  • the annular insulating ceramic sheet 31 in the migration chamber 3 has a high thermal conductivity, which can shorten the cold start time of the machine.
  • Solder can be made of high melting point solder, which eliminates the use of non-heat-resistant materials and high-temperature trace volatile materials. Therefore, the migration tube can work at a temperature of 250 ° C and above, which can more effectively deal with the detection of high-boiling prohibited items such as drugs and explosives. , and can improve the cleaning speed of the system.
  • the surface of the annular insulating ceramic sheet 31 in the preform of the ceramic migration tube to be welded is metallized and treated with hydrogen.
  • the surface of the annular metal electrode sheet 32 in the preform of the ceramic migration tube to be welded is cleaned and nickel-plated and treated with hydrogen. In this way, the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32 are easily welded together by solder.
  • the method for manufacturing a ceramic migration tube can also be provided with a mounting tool.
  • the mounting tool coaxially fixes the plurality of annular insulating ceramic sheets 31 and the plurality of annular metal electrode sheets 32 in the preform of the ceramic migration tube to be welded.
  • a suitable width and thickness of solder is placed between the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32, and a mounting tool is used to position it to ensure that the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32 are coaxial during the mounting process. Fasten.
  • a silver-copper alloy can be used as the solder.
  • a 72:8 silver-copper alloy can be used for the solder, the ratio of silver and copper is 72:8, the solidus is 779°C, and the melting point is 810°C.
  • the first preset heating rate may be equal to or less than 20°C/min.
  • the first preset temperature may be set to 780°C.
  • the first preset time period may be set to 20min.
  • the second preset heating rate may be set to 1-4°C/min.
  • the second preset temperature may be set as the melting point temperature of 810°C.
  • the second preset time period may be set to 1 min.
  • the third preset cooling rate may be equal to or less than 30°C/min.
  • the third preset temperature is 500°C.
  • the hydrogen brazing furnace can naturally cool down to the fourth preset temperature.
  • the fourth preset temperature may be equal to or less than 200°C.
  • the hydrogen brazing furnace is cooled to the fourth preset temperature and the hydrogen supply in the hydrogen brazing furnace is stopped, pressure resistance and air tightness testing of the obtained ceramic migration tube can be performed. If the leakage rate of the tube body is not higher than 1.5 ⁇ 10 -8 Pa ⁇ m3/s, and the withstand voltage value between electrodes is better than 5 ⁇ 10 5 V/cm, the leakage and withstand voltage requirements of the mobility spectrometer equipment are met.

Abstract

The present application relates to the technical field of trace detection, and in particular relates to a ceramic transfer tube and a fabrication method therefor. The ceramic transfer tube comprises: a transfer chamber; an ionization chamber, which is disposed at one end of the transfer chamber; a Faraday cup assembly, which is disposed at the other end of the transfer chamber; an ion gate assembly, which is disposed between the ionization chamber and the transfer chamber; and a suppressor grid, which is disposed between the transfer chamber and the Faraday cup assembly, wherein the transfer chamber comprises a plurality of annular insulating ceramic sheets and a plurality of annular metal electrode sheets, the annular insulating ceramic sheets and the annular metal electrode sheets are alternately arranged in sequence, and adjacent annular insulating ceramic sheets and annular metal electrode sheets are sealed and welded. Compared to the prior art, the annular insulating ceramic sheets and the annular metal electrode sheets in the transfer chamber are alternately arranged in sequence, and the adjacent annular insulating ceramic sheets and annular metal electrode sheets are sealed and welded, which is convenient for installation and allows for low fabrication costs, good sealing performance, a reliable and firm connection, high mechanical strength, and strong shock resistance, which thus improves system stability.

Description

一种陶瓷迁移管及其制作方法A kind of ceramic transfer tube and its making method 技术领域technical field
本申请涉及痕量探测技术领域,尤其涉及一种陶瓷迁移管及其制作方法。The present application relates to the technical field of trace detection, and in particular, to a ceramic migration tube and a manufacturing method thereof.
背景技术Background technique
离子迁移谱仪具有灵敏、快速、功耗低、便携等的优点,是目前国际上反恐、缉毒等领域用于痕量物质现场检测的主流技术。利用离子迁移检测技术大大加强了边防、海关、民航等重要关口对人员和行李的监测力度,有效的打击了走私、贩毒和恐怖袭击活动的实施。Ion mobility spectrometer has the advantages of sensitivity, rapidity, low power consumption and portability. The use of ion migration detection technology has greatly strengthened the monitoring of personnel and luggage at important borders such as border defense, customs, and civil aviation, and effectively combated the implementation of smuggling, drug trafficking and terrorist attacks.
迁移管是离子迁移谱仪的核心器件,也是决定迁移谱仪分离和检测的关键因素。现有商用离子迁移谱仪的迁移管主要采用聚酰亚胺/聚四氟/匹克等绝缘材料与金属电极通过螺母、弹簧及O形密封圈压接而成。The migration tube is the core component of the ion mobility spectrometer, and it is also the key factor determining the separation and detection of the mobility spectrometer. The migration tube of the existing commercial ion mobility spectrometer is mainly made of insulating materials such as polyimide/polytetrafluoro/peak and metal electrodes by crimping with nuts, springs and O-rings.
现有商用离子迁移谱仪的迁移管,装配和密封困难,费时费力,制造成本高,不利于离子迁移谱仪的批量化生产和提高系统稳定性。The migration tube of the existing commercial ion mobility spectrometer is difficult to assemble and seal, time-consuming and laborious, and has a high manufacturing cost, which is not conducive to the mass production of the ion mobility spectrometer and the improvement of system stability.
此外,大部分毒品和爆炸物的沸点都比较高(高于250℃),检测过程中要获得更好的检测效果和更快的清洁速度需要将迁移管温度设置在更高的工作温度。然而,无论是聚酰亚胺、聚四氟还是匹克均难以工作在超过200℃的工作温度,且该类迁移管在高温还会产生痕量释放、多次的冷热冲击也会影响迁移管的密封性进而影响离子迁移谱仪的正常使用。In addition, most drugs and explosives have relatively high boiling points (above 250°C), and to obtain better detection effect and faster cleaning speed during the detection process, the temperature of the migration tube needs to be set at a higher working temperature. However, whether it is polyimide, polytetrafluoroethylene or peak, it is difficult to work at a working temperature of more than 200 °C, and this type of migration tube will produce trace releases at high temperatures, and multiple thermal shocks will also affect the migration tube. The tightness will affect the normal use of the ion mobility spectrometer.
发明内容SUMMARY OF THE INVENTION
有鉴于此,本申请提供了一种陶瓷迁移管及其制作方法,用以解决现有迁移管装配和密封困难、费时费力、制造成本高的问题。In view of this, the present application provides a ceramic transfer tube and a manufacturing method thereof, so as to solve the problems of difficult assembly and sealing of the existing transfer tube, time-consuming and labor-intensive, and high manufacturing cost.
根据本申请的第一方面,提供了一种陶瓷迁移管。该陶瓷迁移管包括:According to a first aspect of the present application, a ceramic migration tube is provided. The ceramic transfer tube includes:
迁移室;migration room;
电离室,所述电离室设置在所述迁移室的一端;an ionization chamber, the ionization chamber is arranged at one end of the migration chamber;
法拉第杯组件,所述法拉第杯组件设置在所述迁移室的另一端;a Faraday cup assembly, the Faraday cup assembly is disposed at the other end of the migration chamber;
离子门组件,所述离子门组件设置在所述电离室与所述迁移室之间;以及an ion gate assembly disposed between the ionization chamber and the migration chamber; and
抑制栅,所述抑制栅设置在所述迁移室与所述法拉第杯组件之间;a suppression grid disposed between the migration chamber and the Faraday cup assembly;
其中,所述迁移室包括多个环形绝缘陶瓷片和多个环形金属电极片,所述环形绝缘陶瓷片与所述环形金属电极片依次交替排列,相邻的所述环形绝缘陶瓷片与所述环形金属电极片密封焊接。Wherein, the migration chamber includes a plurality of annular insulating ceramic sheets and a plurality of annular metal electrode sheets, the annular insulating ceramic sheets and the annular metal electrode sheets are alternately arranged in sequence, and the adjacent annular insulating ceramic sheets and the The annular metal electrode sheet is sealed and welded.
可选地,所述环形绝缘陶瓷片与所述环形金属电极片通过焊料焊接固定,所述环形金属电极片的膨胀系数等于或者接近于所述环形绝缘陶瓷片的膨胀系数。Optionally, the annular insulating ceramic sheet and the annular metal electrode sheet are fixed by soldering, and the expansion coefficient of the annular metal electrode sheet is equal to or close to the expansion coefficient of the annular insulating ceramic sheet.
可选地,所述环形绝缘陶瓷片采用95瓷或者99瓷,所述环形绝缘陶瓷片厚度为1mm-3mm;和/或,Optionally, the annular insulating ceramic sheet is made of 95 porcelain or 99 porcelain, and the annular insulating ceramic sheet has a thickness of 1 mm-3 mm; and/or,
所述环形金属电极片采用可伐合金,所述环形金属电极片厚度为1mm-3mm,和/或,The annular metal electrode sheet adopts Kovar alloy, the thickness of the annular metal electrode sheet is 1mm-3mm, and/or,
所述焊料采用银铜合金。The solder is silver-copper alloy.
可选地,所述环形绝缘陶瓷片表面金属化并烧氢处理,所述环形金属电极片表面经清洗镀镍并烧氢处理。Optionally, the surface of the annular insulating ceramic sheet is metallized and treated with hydrogen burning, and the surface of the annular metal electrode sheet is cleaned and nickel-plated and treated with hydrogen burning.
可选地,所述电离室包括源座、C形弹片和片状电离源,所述源座上贯通设置有中空孔,所述C形弹片过盈配合固定在所述中空孔中,所述片状电离源采用溅射或蒸镀方式沉积在所述C形弹片内壁上;Optionally, the ionization chamber includes a source seat, a C-shaped shrapnel, and a sheet-shaped ionization source, the source seat is provided with a hollow hole therethrough, and the C-shaped shrapnel is fixed in the hollow hole with an interference fit, and the The flake ionization source is deposited on the inner wall of the C-shaped shrapnel by sputtering or evaporation;
在所述中空孔内壁上突出设置有限位凸台,用于轴向顶挡所述C形弹片;A limiting boss is protrudingly arranged on the inner wall of the hollow hole for axially blocking the C-shaped shrapnel;
在所述中空孔的径向一侧设置有夹取凹槽,用于夹取安装或者拆卸所述C形弹片。A clamping groove is provided on the radial side of the hollow hole for clamping, installing or dismounting the C-shaped elastic piece.
可选地,所述离子门组件包括第一离子门栅、陶瓷隔离片和第二离子门栅;所述陶瓷隔离片设置在所述第一离子门栅与所述第二离子门栅之间,用于使所述第一离子门栅与所述第二离子门栅间隔设定距离;所述陶瓷隔离片与所述第一离子门栅及所述第二离子门栅之间密封焊接。Optionally, the ion gate assembly includes a first ion gate grid, a ceramic spacer, and a second ion gate; the ceramic spacer is arranged between the first ion gate and the second ion gate is used to separate the first ion gate and the second ion gate by a set distance; the ceramic spacer is sealed and welded with the first ion gate and the second ion gate.
可选地,所述法拉第杯组件包括法拉第杯和套状在所述法拉第杯上的陶瓷屏蔽罩;所述法拉第杯表面抛光并镀金,以减小探测器噪声;所述陶瓷屏蔽罩外圈金属化处理,焊接后与所述抑制栅等电位,用于屏蔽外界信号对所述法拉第杯信号的干扰;所述法拉第杯通过连接杆与所述陶瓷屏蔽罩密封焊接。Optionally, the Faraday cup assembly includes a Faraday cup and a ceramic shielding cover sleeved on the Faraday cup; the surface of the Faraday cup is polished and plated with gold to reduce detector noise; the ceramic shielding cover has a metal outer ring After welding, it is equipotential with the suppression grid to shield the interference of external signals to the Faraday cup signal; the Faraday cup is sealed and welded with the ceramic shielding cover through a connecting rod.
根据本申请的第二方面,提供了一种陶瓷迁移管制作方法。该陶瓷迁移管制作方法包括:According to a second aspect of the present application, a method for manufacturing a ceramic transfer tube is provided. The manufacturing method of the ceramic migration tube includes:
提供待焊陶瓷迁移管预制件,所述待焊陶瓷迁移管预制件包括多个环形绝缘陶瓷片和多个环形金属电极片,所述环形绝缘陶瓷片与所述环形金属电极片依次交替排列,相邻所述环形绝缘陶瓷片与所述环形金属电极片之间设置有焊料;A ceramic migration tube preform to be welded is provided, the ceramic migration tube preform to be welded includes a plurality of annular insulating ceramic sheets and a plurality of annular metal electrode sheets, the annular insulating ceramic sheets and the annular metal electrode sheets are alternately arranged in sequence, Solder is arranged between the adjacent annular insulating ceramic sheet and the annular metal electrode sheet;
将所述待焊陶瓷迁移管预制件放置于氢钎焊炉中,在氢气保护氛围下以第一预设升温速率将所述氢钎焊炉升温至第一预设温度,并保温第一预设时间段,其中所述第一预设温度小于所述焊料熔点;The ceramic migration tube preform to be welded is placed in a hydrogen brazing furnace, and the hydrogen brazing furnace is heated to a first preset temperature at a first preset heating rate under a hydrogen protective atmosphere, and the first preset temperature is maintained. setting a time period, wherein the first preset temperature is less than the melting point of the solder;
以第二预设升温速率将所述氢钎焊炉升温至第二预设温度,并保温第二预设时间段,其中所述第二预设温度大于或等于所述焊料熔点,所述第二预设升温速率小于所述第一预设升温速率;The hydrogen brazing furnace is heated to a second preset temperature at a second preset heating rate, and maintained for a second preset time period, wherein the second preset temperature is greater than or equal to the melting point of the solder, and the first preset temperature is greater than or equal to the melting point of the solder. 2. The preset heating rate is less than the first preset heating rate;
以第三预设降温速率将所述氢钎焊炉降温至第三预设温度;cooling the hydrogen brazing furnace to a third preset temperature at a third preset cooling rate;
将所述氢钎焊炉降温至第四预设温度,并停止所述氢钎焊炉中的氢气供给。The temperature of the hydrogen brazing furnace is lowered to a fourth preset temperature, and the hydrogen supply in the hydrogen brazing furnace is stopped.
可选地,所述待焊陶瓷迁移管预制件中的所述环形绝缘陶瓷片表面金属化并烧氢处理,所述待焊陶瓷迁移管预制件中的所述环形金属电极片表面经清洗镀镍并烧氢处理,所述焊料采用银铜合金。Optionally, the surface of the annular insulating ceramic sheet in the preform of the ceramic migration tube to be welded is metallized and hydrogen-fired, and the surface of the annular metal electrode sheet in the preform of the ceramic migration tube to be welded is cleaned and plated. Nickel and hydrogen-burning treatment, the solder uses a silver-copper alloy.
可选地,还提供有装架工具,所述装架工具将所述待焊陶瓷迁移管预制件中的所述多个环形绝缘陶瓷片和所述多个环形金属电极片同轴固定。Optionally, a mounting tool is also provided, and the mounting tool coaxially fixes the plurality of annular insulating ceramic sheets and the plurality of annular metal electrode sheets in the ceramic migration tube preform to be welded.
应当理解的是,以上的一般描述和后文的细节描述仅是示例性的,并不能限制本申请。It is to be understood that the foregoing general description and the following detailed description are exemplary only and do not limit the application.
附图说明Description of drawings
为了更清楚地说明本申请具体实施方式或现有技术中的技术方案,下面将对具体实施方式或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图是本申请的一些实施方式,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the specific embodiments of the present application or the technical solutions in the prior art, the accompanying drawings required in the description of the specific embodiments or the prior art will be briefly introduced below. The drawings are some embodiments of the present application. For those of ordinary skill in the art, other drawings can also be obtained from these drawings without any creative effort.
图1为本申请实施例所提供的陶瓷迁移管的剖视图。FIG. 1 is a cross-sectional view of a ceramic migration tube provided by an embodiment of the present application.
图2为图1中电离室的结构示意图。FIG. 2 is a schematic structural diagram of the ionization chamber in FIG. 1 .
图3为图1中离子门组件的分解示意图。FIG. 3 is an exploded schematic view of the ion gate assembly in FIG. 1 .
图4为图1中环形绝缘陶瓷片的结构示意图。FIG. 4 is a schematic structural diagram of the annular insulating ceramic sheet in FIG. 1 .
图5为图1中环形金属电极片的结构示意图。FIG. 5 is a schematic structural diagram of the annular metal electrode sheet in FIG. 1 .
图6为图1中抑制栅及法拉第杯组件的结构示意图。FIG. 6 is a schematic structural diagram of the suppression grid and the Faraday cup assembly in FIG. 1 .
附图标记:Reference number:
1-电离室;1 - ionization chamber;
11-源座;11 - source seat;
111-中空孔;111-Hollow hole;
112-限位凸台;112-Limiting boss;
113-夹取凹槽;113-Clamping groove;
12-C形弹片;12-C-shaped shrapnel;
13-片状电离源;13- Flake ionization source;
2-离子门组件;2- ion gate assembly;
21-第一离子门栅;21-The first ion gate;
22-陶瓷隔离片;22-ceramic spacer;
23-第二离子门栅;23 - the second ion gate;
3-迁移室;3- Migration room;
31-环形绝缘陶瓷片;31-ring insulating ceramic sheet;
32-环形金属电极片;32-ring metal electrode sheet;
4-抑制栅;4-Suppression grid;
5-法拉第杯组件;5- Faraday cup assembly;
51-法拉第杯;51 - Faraday Cup;
52-陶瓷屏蔽罩。52-Ceramic shield.
此处的附图被并入说明书中并构成本说明书的一部分,示出了符合本申请的实施例,并与说明书一起用于解释本申请的原理。The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description serve to explain the principles of the application.
具体实施方式Detailed ways
下面将结合附图对本申请的技术方案进行清楚、完整地描述,显然,所描述的实施例是本申请一部分实施例,而不是全部的实施例。基于本申请中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本申请保护的范围。The technical solutions of the present application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are part of the embodiments of the present application, but not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present application.
在本申请实施例中使用的术语是仅仅出于描述特定实施例的目的,而非旨在限制 本申请。在本申请实施例和所附权利要求书中所使用的单数形式的“一种”、“所述”和“该”也旨在包括多数形式,除非上下文清楚地表示其他含义。The terms used in the embodiments of the present application are only for the purpose of describing specific embodiments, and are not intended to limit the present application. As used in the embodiments of this application and the appended claims, the singular forms "a," "the," and "the" are intended to include the plural forms as well, unless the context clearly dictates otherwise.
应当理解,本文中使用的术语“和/或”仅仅是一种描述关联对象的关联关系,表示可以存在三种关系,例如,A和/或B,可以表示:单独存在A,同时存在A和B,单独存在B这三种情况。另外,本文中字符“/”,一般表示前后关联对象是一种“或”的关系。It should be understood that the term "and/or" used in this document is only an association relationship to describe the associated objects, indicating that there may be three kinds of relationships, for example, A and/or B, which may indicate that A exists alone, and A and B exist at the same time. B, there are three cases of B alone. In addition, the character "/" in this document generally indicates that the related objects are an "or" relationship.
需要注意的是,本申请实施例所描述的“上”、“下”、“左”、“右”等方位词是以附图所示的角度来进行描述的,不应理解为对本申请实施例的限定。此外,在上下文中,还需要理解的是,当提到一个元件连接在另一个元件“上”或者“下”时,其不仅能够直接连接在另一个元件“上”或者“下”,也可以通过中间元件间接连接在另一个元件“上”或者“下”。It should be noted that the directional words such as "up", "down", "left", and "right" described in the embodiments of the present application are described from the angles shown in the drawings, and should not be construed as implementing the present application. Example limitation. Also, in this context, it should also be understood that when an element is referred to as being "on" or "under" another element, it can not only be directly connected "on" or "under" the other element, but also Indirectly connected "on" or "under" another element through intervening elements.
如图1所示,本申请实施例提供了一种陶瓷迁移管。该陶瓷迁移管包括迁移室3、电离室1、法拉第杯组件5、离子门组件2以及抑制栅4。As shown in FIG. 1 , an embodiment of the present application provides a ceramic migration tube. The ceramic migration tube includes a migration chamber 3 , an ionization chamber 1 , a Faraday cup assembly 5 , an ion gate assembly 2 and a suppression grid 4 .
迁移室3用于提供均匀的弱漂移电场和电中性的逆向流场使迁移率,不同的离子群在迁移室3区得到分离。The migration chamber 3 is used to provide a uniform weak drift electric field and an electrically neutral reverse flow field so that the mobility and different ion groups are separated in the region of the migration chamber 3 .
电离室1设置在迁移室3的一端,电离室1用于提供用于离化样品分子或者其它分子的电离能和离化空间。The ionization chamber 1 is arranged at one end of the migration chamber 3, and the ionization chamber 1 is used for providing ionization energy and ionization space for ionizing sample molecules or other molecules.
离子门组件2设置在电离室1与迁移室3之间,离子门组件2用于提供离子的加速电场/截止电场和迁移时钟信号。The ion gate assembly 2 is arranged between the ionization chamber 1 and the migration chamber 3, and the ion gate assembly 2 is used to provide an acceleration electric field/cut-off electric field of the ions and a migration clock signal.
法拉第杯组件5设置在迁移室3的另一端,法拉第杯组件5用于探测离子并产生离子信号。经迁移室3分离的离子群先后到达法拉第杯组件,产生离子信号。The Faraday cup assembly 5 is disposed at the other end of the migration chamber 3, and the Faraday cup assembly 5 is used to detect ions and generate ion signals. The ion groups separated by the migration chamber 3 reach the Faraday cup assembly successively to generate ion signals.
抑制栅4设置在迁移室3与法拉第杯组件5之间,抑制栅4用于屏蔽离子门脉冲电压对法拉第杯组件信号的干扰。The suppression grid 4 is arranged between the migration chamber 3 and the Faraday cup assembly 5, and the suppression grid 4 is used to shield the interference of the ion gate pulse voltage to the signal of the Faraday cup assembly.
如图1、图4和图5所示,迁移室3包括多个环形绝缘陶瓷片31和多个环形金属电极片32。环形绝缘陶瓷片31与环形金属电极片32依次交替排列。相邻的环形绝缘陶瓷片31与环形金属电极片32密封焊接。具体地,多个环形绝缘陶瓷片31依次间隔排列,每两个环形绝缘陶瓷片31之间设置有一个环形金属电极片32,该环形金属电极片32与其相邻的两个环形绝缘陶瓷片31密封焊接在一起。As shown in FIGS. 1 , 4 and 5 , the migration chamber 3 includes a plurality of annular insulating ceramic sheets 31 and a plurality of annular metal electrode sheets 32 . The annular insulating ceramic sheets 31 and the annular metal electrode sheets 32 are arranged alternately in sequence. The adjacent annular insulating ceramic sheets 31 are sealed and welded to the annular metal electrode sheet 32 . Specifically, a plurality of annular insulating ceramic sheets 31 are arranged at intervals in sequence, and an annular metal electrode sheet 32 is disposed between every two annular insulating ceramic sheets 31 , and the annular metal electrode sheet 32 is adjacent to two annular insulating ceramic sheets 31 . Seal welded together.
迁移室3中的环形绝缘陶瓷片31与环形金属电极片32依次交替排列,相邻的环 形绝缘陶瓷片31与环形金属电极片32密封焊接,安装方便,制造成本低;密封性能佳,连接可靠牢固,机械强度高,抗震性能强,提高了系统稳定性。迁移室3中的环形绝缘陶瓷片31导热系数较高,可缩短机器的冷启动时间。The annular insulating ceramic sheets 31 and the annular metal electrode sheets 32 in the migration chamber 3 are arranged alternately in turn, and the adjacent annular insulating ceramic sheets 31 and the annular metal electrode sheet 32 are sealed and welded, which is convenient for installation and low in manufacturing cost; good sealing performance and reliable connection Firm, high mechanical strength, strong shock resistance, improve system stability. The annular insulating ceramic sheet 31 in the migration chamber 3 has a high thermal conductivity, which can shorten the cold start time of the machine.
相邻环形绝缘陶瓷片31与环形金属电极片32之间的密封焊接结构可根据需要具体设置。作为优选,环形绝缘陶瓷片31与环形金属电极片32可以通过焊料焊接固定。环形金属电极片32的膨胀系数可等于或者接近于环形绝缘陶瓷片31的膨胀系数。The sealing and welding structure between the adjacent annular insulating ceramic sheets 31 and the annular metal electrode sheet 32 can be specifically set as required. Preferably, the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32 can be fixed by soldering. The expansion coefficient of the annular metal electrode sheet 32 may be equal to or close to the expansion coefficient of the annular insulating ceramic sheet 31 .
焊料可采用高熔点焊料,杜绝了非耐热材料和高温痕量挥发材料的使用,因此迁移管可工作在250℃及以上温度,可更有效的应对毒品、爆炸物等高沸点违禁物品的检测,并能提高系统的清洁速度。Solder can be made of high melting point solder, which eliminates the use of non-heat-resistant materials and high-temperature trace volatile materials. Therefore, the migration tube can work at a temperature of 250 ° C and above, which can more effectively deal with the detection of high-boiling prohibited items such as drugs and explosives. , and can improve the cleaning speed of the system.
环形绝缘陶瓷片31、环形金属电极片32及焊料的材料及厚度具体选用应考虑其可焊接性和焊接稳定性。The materials and thicknesses of the annular insulating ceramic sheet 31 , the annular metal electrode sheet 32 and the solder should be selected in consideration of their weldability and welding stability.
更优选地,如图4所示,环形绝缘陶瓷片31采用95瓷或者99瓷。环形绝缘陶瓷片31具体可设置厚度为1mm-3mm。More preferably, as shown in FIG. 4 , the annular insulating ceramic sheet 31 adopts 95 porcelain or 99 porcelain. Specifically, the annular insulating ceramic sheet 31 may have a thickness of 1mm-3mm.
如图5所示,环形金属电极片32可采用可伐合金。可伐合金与环形绝缘陶瓷片31的膨胀系数相接近。可伐合金的厚度可设置为1mm-3mm。例如,环形金属电极片32可采用4J33可伐合金。As shown in FIG. 5 , the annular metal electrode sheet 32 can be made of Kovar alloy. The coefficient of expansion of the Kovar alloy is close to that of the annular insulating ceramic sheet 31 . The thickness of Kovar alloy can be set to 1mm-3mm. For example, the annular metal electrode sheet 32 can be made of 4J33 Kovar alloy.
焊料可采用银铜合金。铜银合金熔点高,允许迁移管可工作在较高温度,可更有效的应对毒品、爆炸物等高沸点违禁物品的检测,并能提高系统的清洁速度。具体地,焊料采用72:8银铜合金,银、铜比例为72:8,其固相线为779℃,熔点为810℃。The solder can be silver-copper alloy. The high melting point of copper-silver alloy allows the migration tube to work at a higher temperature, which can more effectively deal with the detection of high-boiling prohibited items such as drugs and explosives, and can improve the cleaning speed of the system. Specifically, a 72:8 silver-copper alloy was used as the solder, the ratio of silver to copper was 72:8, the solidus was 779°C, and the melting point was 810°C.
电离室的具体结构可根据需要设置,其能提供用于离化样品分子或者其它分子的电离能和离化空间即可。作为优选,如图2所示,电离室13包括电离源和源座11。源座11用于安装和固定电离源13,其具体结构可根据电离源13的具体结构来设置。电离源13可采用放射源如63Ni、3H也可以使用非放射源如UV、DBD(介质阻挡放电)及电晕放电电离源等。The specific structure of the ionization chamber can be set as required, as long as it can provide ionization energy and ionization space for ionizing sample molecules or other molecules. Preferably, as shown in FIG. 2 , the ionization chamber 13 includes an ionization source and a source base 11 . The source seat 11 is used for installing and fixing the ionization source 13 , and its specific structure can be set according to the specific structure of the ionization source 13 . The ionization source 13 can use radioactive sources such as 63Ni, 3H, or non-radioactive sources such as UV, DBD (Dielectric Barrier Discharge) and corona discharge ionization sources.
具体地,如图2所示,电离室1可包括源座11、C形弹片12和片状电离源13。源座11为环形结构,其上贯通设置有中空孔111。C形弹片12具有弹性,其受力时能发生弹性变形。C形弹片12过盈配合固定在中空孔111中。C形弹片12可向其径向内侧发生弹性变形,并与源座11中空孔111内壁相抵。片状电离源13可采用溅射方式或者蒸镀方式或者其他方式沉积在C形弹片12内壁上。Specifically, as shown in FIG. 2 , the ionization chamber 1 may include a source seat 11 , a C-shaped elastic sheet 12 and a sheet-shaped ionization source 13 . The source seat 11 is an annular structure, and a hollow hole 111 is formed therethrough. The C-shaped elastic piece 12 has elasticity, and can be elastically deformed when it is stressed. The C-shaped elastic piece 12 is fixed in the hollow hole 111 by interference fit. The C-shaped elastic piece 12 can be elastically deformed toward the inner side of the radial direction thereof, and abuts against the inner wall of the hollow hole 111 of the source seat 11 . The sheet-shaped ionization source 13 can be deposited on the inner wall of the C-shaped elastic sheet 12 by sputtering, vapor deposition or other methods.
在中空孔111内壁上可突出设置有限位凸台112,用于轴向顶挡C形弹片12。将C形弹片12放置于源座11中空孔111内时,限位凸台112可顶挡C形弹片12,以阻止C形弹片12继续插入并提示C形弹片12及片状电离源13安装到位限制及提示放射源安装到位。A limiting boss 112 can be protruded from the inner wall of the hollow hole 111 for axially topping off the C-shaped elastic piece 12 . When the C-shaped shrapnel 12 is placed in the hollow hole 111 of the source base 11, the limiting boss 112 can block the C-shaped shrapnel 12 to prevent the C-shaped shrapnel 12 from continuing to be inserted and prompt the C-shaped shrapnel 12 and the ionization source 13 to be installed In-place restrictions and prompts for radioactive sources to be installed in place.
在中空孔111的径向一侧可设置有夹取凹槽113,夹取凹槽113与中空孔111相连通,可用于夹取安装或者拆卸C形弹片12。A clamping groove 113 may be provided on the radial side of the hollow hole 111 , and the clamping groove 113 communicates with the hollow hole 111 and can be used for clamping, installing or removing the C-shaped elastic piece 12 .
更具体地,片状电离源13可采用63Ni源。C形弹片12对应设置为C形镍基弹片。63Ni源的片状电离源13可蒸镀在C形镍基弹片内壁上。More specifically, the sheet-shaped ionization source 13 may use a 63Ni source. The C-shaped elastic pieces 12 are correspondingly arranged as C-shaped nickel-based elastic pieces. The sheet-shaped ionization source 13 of the 63Ni source can be evaporated on the inner wall of the C-shaped nickel-based elastic sheet.
离子门组件的具体结构可根据需要设置,其能提供离子的加速电场/截止电场和迁移时钟信号即可。作为优选,如图2所示,离子门组件2可包括第一离子门栅21、陶瓷隔离片22和第二离子门栅23。陶瓷隔离片22设置在第一离子门栅21与第二离子门栅23之间,用于使第一离子门栅21与第二离子门栅23间隔设定距离。陶瓷隔离片22与第一离子门栅21及第二离子门栅23之间密封焊接,可防止熔融焊料溅散/溢出降低离子门间的绝缘性。更优选地,陶瓷隔离片22不超过0.7mm,用于隔离第一离子门栅21与第二离子门栅23。对应地,第一离子门栅21与第二离子门栅23间隔距离不超过0.7mm。The specific structure of the ion gate assembly can be set as required, as long as it can provide the acceleration electric field/cut-off electric field and the migration clock signal of the ions. Preferably, as shown in FIG. 2 , the ion gate assembly 2 may include a first ion gate grid 21 , a ceramic spacer 22 and a second ion gate grid 23 . The ceramic spacer 22 is disposed between the first ion gate grid 21 and the second ion gate grid 23 , and is used to space the first ion gate grid 21 and the second ion gate grid 23 by a predetermined distance. The ceramic spacer 22 is sealed and welded with the first ion gate grid 21 and the second ion gate grid 23, which can prevent the molten solder from spattering/overflowing and reducing the insulation between the ion gates. More preferably, the ceramic spacer 22 is not more than 0.7 mm for isolating the first ion gate 21 and the second ion gate 23 . Correspondingly, the distance between the first ion gate grid 21 and the second ion gate grid 23 is not more than 0.7 mm.
法拉第杯组件的具体结构可根据需要设置,其能实现探测离子并产生离子信号功能即可。作为优选,如图6所示,法拉第杯组件5可包括法拉第杯51和陶瓷屏蔽罩52。法拉第杯51通过连接杆与陶瓷屏蔽罩52密封焊接。例如图1所示,陶瓷屏蔽罩52可套装在法拉第杯51的连接杆上。法拉第杯51表面抛光并镀金,以减小探测器噪声。陶瓷屏蔽罩52外圈金属化处理,焊接后与抑制栅4等电位,用于屏蔽外界信号对法拉第杯51信号的干扰。The specific structure of the Faraday cup assembly can be set as required, as long as it can detect ions and generate ion signals. Preferably, as shown in FIG. 6 , the Faraday cup assembly 5 may include a Faraday cup 51 and a ceramic shield 52 . The Faraday cup 51 is sealed and welded to the ceramic shield 52 through a connecting rod. For example, as shown in FIG. 1 , the ceramic shield 52 can be fitted over the connecting rod of the Faraday cup 51 . The Faraday cup 51 is polished and gold plated to reduce detector noise. The outer ring of the ceramic shielding cover 52 is metallized, and after welding, it is equipotential with the suppression grid 4, which is used to shield the interference of the external signal to the signal of the Faraday cup 51.
法拉第杯51与陶瓷屏蔽罩52密封焊接。例如,法拉第杯51与与屏蔽罩的封接方式为可在连接法拉第杯51的连杆上嵌套内外圈金属化的环形陶瓷屏蔽罩52,并可采用双层套封方式封接。The Faraday cup 51 is hermetically welded to the ceramic shield 52 . For example, the Faraday cup 51 can be sealed with the shielding cover by nesting the metallized annular ceramic shielding cover 52 on the inner and outer rings on the connecting rod connecting the Faraday cup 51, and sealing with double-layer casing.
抑制栅的具体结构可根据需要设置,其能屏蔽离子门脉冲电压对法拉第杯51信号的干扰即可。作为优选,抑制栅4可设置为片状栅网结构,片状栅网结构具体可设置为六边形、圆形等。The specific structure of the suppression gate can be set as required, as long as it can shield the interference of the pulse voltage of the ion gate to the signal of the Faraday cup 51 . Preferably, the suppression grid 4 can be configured as a sheet-like grid structure, and the sheet-like grid structure can be specifically configured as a hexagon, a circle, or the like.
根据同一发明构思,本申请还提供了一种陶瓷迁移管制作方法。如图1所示,该 陶瓷迁移管制作方法包括:According to the same inventive concept, the present application also provides a method for manufacturing a ceramic transfer tube. As shown in Figure 1, the manufacturing method of the ceramic migration tube includes:
首先,提供待焊陶瓷迁移管预制件。该待焊陶瓷迁移管预制件包括多个环形绝缘陶瓷片31和多个环形金属电极片32,环形绝缘陶瓷片31与环形金属电极片32依次交替排列,相邻环形绝缘陶瓷片31与环形金属电极片32之间设置有焊料。First, a preform of a ceramic migration tube to be welded is provided. The ceramic migration tube preform to be welded includes a plurality of annular insulating ceramic sheets 31 and a plurality of annular metal electrode sheets 32 . Solder is provided between the electrode pads 32 .
然后,将待焊陶瓷迁移管预制件放置于氢钎焊炉中,在氢气保护氛围下以第一预设升温速率将氢钎焊炉升温至第一预设温度,并保温第一预设时间段,以确保焊件温度均匀。其中第一预设温度小于焊料的熔点。Then, the ceramic migration tube preform to be welded is placed in a hydrogen brazing furnace, and the hydrogen brazing furnace is heated to a first preset temperature at a first preset heating rate under a hydrogen protective atmosphere, and maintained for a first preset time. section to ensure that the weldment temperature is uniform. The first preset temperature is less than the melting point of the solder.
之后,以第二预设升温速率将氢钎焊炉升温至第二预设温度,并保温第二预设时间段,以确保各焊缝焊料熔融充分、焊接界面浸润良好。其中第二预设温度大于或者等于焊料的熔点,第二预设升温速率小于第一预设升温速率;After that, the hydrogen brazing furnace is heated to a second preset temperature at a second preset heating rate, and maintained for a second preset time period to ensure that the solder of each welding seam is fully melted and the welding interface is well infiltrated. Wherein the second preset temperature is greater than or equal to the melting point of the solder, and the second preset heating rate is less than the first preset heating rate;
之后,以第三预设降温速率将氢钎焊炉降温至第三预设温度,以缓慢释放环形绝缘陶瓷片31与环形金属电极片32之间焊缝的封接应力,防止陶瓷炸裂。After that, the hydrogen brazing furnace is cooled to a third preset temperature at a third preset cooling rate to slowly release the sealing stress of the welding seam between the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32 to prevent the ceramic from bursting.
之后,将氢钎焊炉降温至第四预设温度,并停止氢钎焊炉中的氢气供给。After that, the temperature of the hydrogen brazing furnace is lowered to the fourth preset temperature, and the hydrogen supply in the hydrogen brazing furnace is stopped.
本实施例中的迁移室3中的环形绝缘陶瓷片31与环形金属电极片32依次交替排列,相邻的环形绝缘陶瓷片31与环形金属电极片32通过焊料密封焊接,一体成型,安装方便,制造成本低;密封性能佳,连接可靠牢固,机械强度高,抗震性能强,提高了系统稳定性。迁移室3中的环形绝缘陶瓷片31导热系数较高,可缩短机器的冷启动时间。In this embodiment, the annular insulating ceramic sheets 31 and the annular metal electrode sheets 32 in the migration chamber 3 are alternately arranged in sequence, and the adjacent annular insulating ceramic sheets 31 and the annular metal electrode sheet 32 are sealed and welded by solder, which is integrally formed and easy to install. Low manufacturing cost; good sealing performance, reliable and firm connection, high mechanical strength, strong shock resistance, and improved system stability. The annular insulating ceramic sheet 31 in the migration chamber 3 has a high thermal conductivity, which can shorten the cold start time of the machine.
焊料可采用高熔点焊料,杜绝了非耐热材料和高温痕量挥发材料的使用,因此迁移管可工作在250℃及以上温度,可更有效的应对毒品、爆炸物等高沸点违禁物品的检测,并能提高系统的清洁速度。Solder can be made of high melting point solder, which eliminates the use of non-heat-resistant materials and high-temperature trace volatile materials. Therefore, the migration tube can work at a temperature of 250 ° C and above, which can more effectively deal with the detection of high-boiling prohibited items such as drugs and explosives. , and can improve the cleaning speed of the system.
为使环形绝缘陶瓷片31与环形金属电极片32能更好地密封焊接在一起,作为优选,焊接前,待焊陶瓷迁移管预制件中的环形绝缘陶瓷片31表面金属化并烧氢处理,待焊陶瓷迁移管预制件中的环形金属电极片32表面经清洗镀镍并烧氢处理。如此,环形绝缘陶瓷片31与环形金属电极片32易通过焊料焊接在一起。In order to make the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32 better sealed and welded together, preferably, before welding, the surface of the annular insulating ceramic sheet 31 in the preform of the ceramic migration tube to be welded is metallized and treated with hydrogen. The surface of the annular metal electrode sheet 32 in the preform of the ceramic migration tube to be welded is cleaned and nickel-plated and treated with hydrogen. In this way, the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32 are easily welded together by solder.
为实现焊接稳定性,该陶瓷迁移管制作方法还可以提供有装架工具。装架工具将待焊陶瓷迁移管预制件中的多个环形绝缘陶瓷片31和多个环形金属电极片32同轴固定。具体地,在环形绝缘陶瓷片31与环形金属电极片32之间放入合适宽度及厚度焊料,并用装架工具定位,确保装架过程中环形绝缘陶瓷片31与环形金属电极片32同 轴后紧固。In order to achieve welding stability, the method for manufacturing a ceramic migration tube can also be provided with a mounting tool. The mounting tool coaxially fixes the plurality of annular insulating ceramic sheets 31 and the plurality of annular metal electrode sheets 32 in the preform of the ceramic migration tube to be welded. Specifically, a suitable width and thickness of solder is placed between the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32, and a mounting tool is used to position it to ensure that the annular insulating ceramic sheet 31 and the annular metal electrode sheet 32 are coaxial during the mounting process. Fasten.
作为优选,焊料可采用银铜合金。例如焊料具体可采用72:8银铜合金,银、铜比例为72:8,其固相线为779℃,熔点为810℃。Preferably, a silver-copper alloy can be used as the solder. For example, a 72:8 silver-copper alloy can be used for the solder, the ratio of silver and copper is 72:8, the solidus is 779°C, and the melting point is 810°C.
第一预设升温速率可等于或者小于20℃/min。第一预设温度可设置为780℃。第一预设时间段可设置为20min。The first preset heating rate may be equal to or less than 20°C/min. The first preset temperature may be set to 780°C. The first preset time period may be set to 20min.
第二预设升温速率可设置为1-4℃/min。第二预设温度可设置为熔点温度810℃。第二预设时间段可设置为1min。The second preset heating rate may be set to 1-4°C/min. The second preset temperature may be set as the melting point temperature of 810°C. The second preset time period may be set to 1 min.
第三预设降温速率可等于或者小于30℃/min。第三预设温度为500℃。The third preset cooling rate may be equal to or less than 30°C/min. The third preset temperature is 500°C.
氢钎焊炉可自然降温至第四预设温度。第四预设温度可等于或者小于200℃。The hydrogen brazing furnace can naturally cool down to the fourth preset temperature. The fourth preset temperature may be equal to or less than 200°C.
作为优选,在将氢钎焊炉降温至第四预设温度,并停止氢钎焊炉中的氢气供给之后,可对获得的陶瓷迁移管进行耐压及气密性检测。若管体泄漏率不高于1.5×10 -8Pa·m3/s,极间耐压值优于5×10 5V/cm,则满足迁移谱仪设备泄露和耐压要求。 Preferably, after the hydrogen brazing furnace is cooled to the fourth preset temperature and the hydrogen supply in the hydrogen brazing furnace is stopped, pressure resistance and air tightness testing of the obtained ceramic migration tube can be performed. If the leakage rate of the tube body is not higher than 1.5×10 -8 Pa·m3/s, and the withstand voltage value between electrodes is better than 5×10 5 V/cm, the leakage and withstand voltage requirements of the mobility spectrometer equipment are met.
以上仅为本申请的优选实施例而已,并不用于限制本申请,对于本领域的技术人员来说,本申请可以有各种更改和变化。凡在本申请的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本申请的保护范围之内。The above are only preferred embodiments of the present application, and are not intended to limit the present application. For those skilled in the art, the present application may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of this application shall be included within the protection scope of this application.

Claims (10)

  1. 一种陶瓷迁移管,其特征在于,包括:A ceramic migration tube, characterized in that, comprising:
    迁移室(3);Migration room (3);
    电离室(1),所述电离室(1)设置在所述迁移室(3)的一端;an ionization chamber (1), the ionization chamber (1) is arranged at one end of the migration chamber (3);
    法拉第杯组件(5),所述法拉第杯组件(5)设置在所述迁移室(3)的另一端;a Faraday cup assembly (5), the Faraday cup assembly (5) is arranged at the other end of the migration chamber (3);
    离子门组件(2),所述离子门组件(2)设置在所述电离室(1)与所述迁移室(3)之间;以及an ion gate assembly (2), the ion gate assembly (2) being arranged between the ionization chamber (1) and the migration chamber (3); and
    抑制栅(4),所述抑制栅(4)设置在所述迁移室(3)与所述法拉第杯组件(5)之间;a suppression grid (4), the suppression grid (4) is arranged between the migration chamber (3) and the Faraday cup assembly (5);
    其中,所述迁移室(3)包括多个环形绝缘陶瓷片(31)和多个环形金属电极片(32),所述环形绝缘陶瓷片(31)与所述环形金属电极片(32)依次交替排列,相邻的所述环形绝缘陶瓷片(31)与所述环形金属电极片(32)密封焊接。Wherein, the migration chamber (3) includes a plurality of annular insulating ceramic sheets (31) and a plurality of annular metal electrode sheets (32), and the annular insulating ceramic sheets (31) and the annular metal electrode sheets (32) are in sequence Alternately arranged, the adjacent annular insulating ceramic sheets (31) are sealed and welded to the annular metal electrode sheet (32).
  2. 根据权利要求1所述的陶瓷迁移管,其特征在于,所述环形绝缘陶瓷片(31)与所述环形金属电极片(32)通过焊料焊接固定,所述环形金属电极片(32)的膨胀系数等于或者接近于所述环形绝缘陶瓷片(31)的膨胀系数。The ceramic migration tube according to claim 1, characterized in that, the annular insulating ceramic sheet (31) and the annular metal electrode sheet (32) are fixed by soldering, and the expansion of the annular metal electrode sheet (32) The coefficient is equal to or close to the expansion coefficient of the annular insulating ceramic sheet (31).
  3. 根据权利要求2所述的陶瓷迁移管,其特征在于,所述环形绝缘陶瓷片(31)采用95瓷或者99瓷,所述环形绝缘陶瓷片(31)厚度为1mm-3mm;和/或,The ceramic migration tube according to claim 2, characterized in that, the annular insulating ceramic sheet (31) adopts 95 porcelain or 99 porcelain, and the annular insulating ceramic sheet (31) has a thickness of 1 mm-3 mm; and/or,
    所述环形金属电极片(32)采用可伐合金,所述环形金属电极片(32)厚度为1mm-3mm,和/或,The annular metal electrode sheet (32) adopts Kovar alloy, the thickness of the annular metal electrode sheet (32) is 1 mm-3 mm, and/or,
    所述焊料采用银铜合金。The solder is silver-copper alloy.
  4. 根据权利要求2所述的陶瓷迁移管,其特征在于,所述环形绝缘陶瓷片(31)表面金属化并烧氢处理,所述环形金属电极片(32)表面经清洗镀镍并烧氢处理。The ceramic transfer tube according to claim 2, characterized in that the surface of the annular insulating ceramic sheet (31) is metallized and subjected to hydrogen-burning treatment, and the surface of the annular metal electrode sheet (32) is cleaned and nickel-plated and subjected to hydrogen-burning treatment .
  5. 根据权利要求1所述的陶瓷迁移管,其特征在于,所述电离室(1)包括源座(11)、C形弹片(12)和片状电离源(13),所述源座(11)上贯通设置有中空孔(111),所述C形弹片(12)过盈配合固定在所述中空孔(111)中,所述片状电离源(13)采用溅射或蒸镀方式沉积在所述C形弹片(12)内壁上;The ceramic transfer tube according to claim 1, characterized in that, the ionization chamber (1) comprises a source seat (11), a C-shaped elastic piece (12) and a sheet-shaped ionization source (13), the source seat (11) ) is provided with a hollow hole (111) through it, the C-shaped elastic sheet (12) is fixed in the hollow hole (111) with interference fit, and the sheet-shaped ionization source (13) is deposited by sputtering or evaporation on the inner wall of the C-shaped shrapnel (12);
    在所述中空孔(111)内壁上突出设置有限位凸台(112),用于轴向顶挡所述C形弹片(12);A limiting boss (112) is protruded on the inner wall of the hollow hole (111) for axially blocking the C-shaped elastic piece (12);
    在所述中空孔(111)的径向一侧设置有夹取凹槽(113),用于夹取安装或者拆 卸所述C形弹片(12)。A clamping groove (113) is provided on the radial side of the hollow hole (111) for clamping, installing or dismounting the C-shaped elastic piece (12).
  6. 根据权利要求1所述的陶瓷迁移管,其特征在于,所述离子门组件(2)包括第一离子门栅(21)、陶瓷隔离片(22)和第二离子门栅(23);所述陶瓷隔离片(22)设置在所述第一离子门栅(21)与所述第二离子门栅(23)之间,用于使所述第一离子门栅(21)与所述第二离子门栅(23)间隔设定距离;所述陶瓷隔离片(22)与所述第一离子门栅(21)及所述第二离子门栅(23)之间密封焊接。The ceramic migration tube according to claim 1, wherein the ion gate assembly (2) comprises a first ion gate grid (21), a ceramic spacer (22) and a second ion gate grid (23); the The ceramic spacer (22) is arranged between the first ion gate grid (21) and the second ion gate grid (23), and is used for connecting the first ion gate grid (21) and the second ion gate grid (21) with the second ion gate grid (23). The two ion gate grids (23) are separated by a set distance; the ceramic spacer (22) is sealed and welded with the first ion gate grid (21) and the second ion gate grid (23).
  7. 根据权利要求1所述的陶瓷迁移管,其特征在于,所述法拉第杯组件(5)包括法拉第杯(51)和套装在所述法拉第杯(51)上的陶瓷屏蔽罩(52);所述法拉第杯(51)表面抛光并镀金,以减小探测器噪声;所述陶瓷屏蔽罩(52)外圈金属化处理,焊接后与所述抑制栅(4)等电位,用于屏蔽外界信号对所述法拉第杯信号的干扰;所述法拉第杯(51)通过连接杆与所述陶瓷屏蔽罩(52)密封焊接。The ceramic migration tube according to claim 1, wherein the Faraday cup assembly (5) comprises a Faraday cup (51) and a ceramic shield (52) sleeved on the Faraday cup (51); the The surface of the Faraday cup (51) is polished and plated with gold to reduce the noise of the detector; the outer ring of the ceramic shield (52) is metallized, and after welding, it is equipotential with the suppression grid (4) to shield the external signal against the The interference of the Faraday cup signal; the Faraday cup (51) is sealed and welded with the ceramic shielding cover (52) through a connecting rod.
  8. 一种陶瓷迁移管制作方法,其特征在于,包括:A method for manufacturing a ceramic transfer tube, comprising:
    提供待焊陶瓷迁移管预制件,所述待焊陶瓷迁移管预制件包括多个环形绝缘陶瓷片(31)和多个环形金属电极片(32),所述环形绝缘陶瓷片(31)与所述环形金属电极片(32)依次交替排列,相邻所述环形绝缘陶瓷片(31)与所述环形金属电极片(32)之间设置有焊料;A ceramic migration tube preform to be welded is provided, the ceramic migration tube preform to be welded includes a plurality of annular insulating ceramic sheets (31) and a plurality of annular metal electrode sheets (32), the annular insulating ceramic sheet (31) and the The annular metal electrode sheets (32) are alternately arranged in sequence, and solder is provided between the adjacent annular insulating ceramic sheets (31) and the annular metal electrode sheet (32);
    将所述待焊陶瓷迁移管预制件放置于氢钎焊炉中,在氢气保护氛围下以第一预设升温速率将所述氢钎焊炉升温至第一预设温度,并保温第一预设时间段,其中所述第一预设温度小于所述焊料熔点;The ceramic migration tube preform to be welded is placed in a hydrogen brazing furnace, and the hydrogen brazing furnace is heated to a first preset temperature at a first preset heating rate under a hydrogen protective atmosphere, and the first preset temperature is maintained. setting a time period, wherein the first preset temperature is less than the melting point of the solder;
    以第二预设升温速率将所述氢钎焊炉升温至第二预设温度,并保温第二预设时间段,其中所述第二预设温度大于或等于所述焊料熔点,所述第二预设升温速率小于所述第一预设升温速率;The hydrogen brazing furnace is heated to a second preset temperature at a second preset heating rate, and maintained for a second preset time period, wherein the second preset temperature is greater than or equal to the melting point of the solder, and the first preset temperature is greater than or equal to the melting point of the solder. 2. The preset heating rate is less than the first preset heating rate;
    以第三预设降温速率将所述氢钎焊炉降温至第三预设温度;cooling the hydrogen brazing furnace to a third preset temperature at a third preset cooling rate;
    将所述氢钎焊炉降温至第四预设温度,并停止所述氢钎焊炉中的氢气供给。The temperature of the hydrogen brazing furnace is lowered to a fourth preset temperature, and the hydrogen supply in the hydrogen brazing furnace is stopped.
  9. 根据权利要求8所述的陶瓷迁移管制作方法,其特征在于,所述待焊陶瓷迁移管预制件中的所述环形绝缘陶瓷片(31)表面金属化并烧氢处理,所述待焊陶瓷迁移管预制件中的所述环形金属电极片(32)表面经清洗镀镍并烧氢处理,所述焊料采用银铜合金。The method for manufacturing a ceramic migration tube according to claim 8, characterized in that, the surface of the annular insulating ceramic sheet (31) in the preform of the ceramic migration tube to be welded is metallized and hydrogen-fired, and the ceramic to be welded The surface of the annular metal electrode sheet (32) in the migration tube preform is cleaned and nickel-plated and treated with hydrogen, and the solder is silver-copper alloy.
  10. 根据权利要求8所述的陶瓷迁移管制作方法,其特征在于,还提供有装架工 具,所述装架工具将所述待焊陶瓷迁移管预制件中的所述多个环形绝缘陶瓷片(31)和所述多个环形金属电极片(32)同轴固定。The method for manufacturing a ceramic migration tube according to claim 8, characterized in that a mounting tool is further provided, and the mounting tool is used to mount the plurality of annular insulating ceramic sheets ( 31) and the plurality of annular metal electrode sheets (32) are coaxially fixed.
PCT/CN2021/115971 2021-01-07 2021-09-01 Ceramic transfer tube and fabrication method therefor WO2022148034A1 (en)

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