Device and method for detecting trace impurities in electronic mixed gas
By combining multiple types of multi-level MOFs sensor detection units with gas chromatographs, the problem of low accuracy in detecting trace impurities in electronic mixed gases in the existing technology has been solved, and high-precision, low-interference impurity detection has been achieved, ensuring the quality of the wafers.
Patent Information
- Application Number
- CN202510677548.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-26
- Publication Date
- 2025-09-26
AI Technical Summary
Existing methods for detecting trace impurities in electronic mixed gases have problems such as complex equipment, high maintenance costs, low detection accuracy, and inability to detect impurities in inert gases, and cannot meet the needs of efficient and high-precision detection.
A variety of multi-level MOFs sensor detection units are combined with a gas chromatograph. The gas is pretreated and multi-level detected through a metal impurity treatment unit, a dehumidification unit, and a gas source replenishment unit. The selective adsorption characteristics of the MOFs sensor are used for precise detection.
It achieves ppb-level detection of impurities in electronic mixed gas, improves detection accuracy and sensitivity, reduces detection interference, extends sensor life, and avoids damage to wafers caused by negative errors.
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Figure CN120703203A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of special gas detection, and in particular to a device and method for detecting trace impurities in electronic mixed gas. Background Art
[0002] Electronic mixed gases are classified by use as follows:
[0003] 1. Doping gas mixtures, such as arsine (AsH3), phosphine (PH3), and diborane (B2H6), are typically mixed with inert gases (such as argon and nitrogen) as carrier gases. They are used in semiconductor doping processes to adjust the conductivity and resistivity of the material.
[0004] 2. Epitaxial growth gas mixture, composed of silane (SiH4), dichlorosilane (SiH2Cl2), silicon tetrachloride (SiCl4), etc., usually with helium, hydrogen, or nitrogen as diluent. Used to deposit single crystal materials such as silicon epitaxial layers or silicon nitride films on the substrate surface.
[0005] 3. Etching gas mixture, which consists of a mixture of fluoride gases (such as CF4, NF3, C2F6) and inert gases (such as argon and oxygen). It is used in dry etching processes to precisely control the surface structure of chips.
[0006] 4. Ion implantation gases, composed of phosphorus (PH3), boron (B2H6), and arsenic (AsH3) gases, usually mixed with helium or hydrogen. Used to adjust semiconductor threshold voltages through high-energy ion implantation.
[0007] 5. Chemical vapor deposition (CVD) gas mixture, consisting of silane (SiH4), ammonia (NH3), oxygen (O2), etc., with nitrogen or argon often used as the balance gas. Used to deposit insulating or conductive films through vapor phase reactions.
[0008] 6. Shielding and diluent gases, consisting of binary or ternary mixtures of inert gases such as argon (Ar), nitrogen (N2), and helium (He) (e.g., Ar-He, Ar-N2, He-N2). These gases are used to prevent oxidation or explosion risks during processes such as welding protection or environmental control during epitaxial growth.
[0009] Electronic gas mixtures are widely used. Shielding and diluent gases are crucial and widely used in semiconductor processes. If these gases contain high levels of impurities, they can react with the wafer and film materials during processes like wafer etching and thin film deposition, potentially causing irreversible damage to the wafer, etching, and circuit deposition processes, potentially rendering the wafers useless. Therefore, controlling the impurity content of these gases is crucial, with a minimum requirement of ppb to minimize damage to the wafers.
[0010] Currently, there are several types of impurity detection methods for electronic mixed gases:
[0011] 1. Gas chromatography (GC) is based on the separation of gas components using a chromatographic column and the quantitative analysis of impurities using detectors (such as FID, TCD, and PDHID). It is primarily used to detect impurities such as H2, O2, N2, and CH4 in high-purity helium (He) and argon (Ar) shielding gases; and to analyze trace amounts of CO, CO2, and H2O in nitrogen (N2) and synthetic air (Ar-O2) diluent gases. Its advantages include high separation efficiency (capable of simultaneously detecting more than 10 impurities with detection limits down to the ppb level (e.g., H2 <1.0ppm)) and flexible configuration (supporting heart-cutting and backflush techniques to prevent detector contamination by high-concentration components). Its disadvantages include complex equipment (requiring a carrier gas purifier and valve system, resulting in high maintenance costs), time-consuming (long sample pretreatment and analysis cycles (>30 minutes per sample)), and the inability to directly detect metallic impurities in permanent gases (such as He and Ar).
[0012] 2. Pulsed Discharge Helium Ionization Detection (PDHID) uses helium plasma to ionize impurity molecules and quantitatively analyze them through current signals. It is primarily used to detect trace impurities such as Ne, H2, and O2 in ultrapure helium (He) as a protective gas (detection limit 0.01 μL / L); and hydrocarbons such as CH4 and C2H2 in high-purity nitrogen (N2) as a diluent gas. Its advantages are ultra-high sensitivity (detection limit as low as 0.01 ppb (e.g., Ne)) and strong versatility (suitable for non-corrosive gases). Its disadvantages are that it is limited to helium carrier gas and cannot be used with other gas systems. It cannot detect inert gases, such as He and Ne, which do not generate signals themselves, and the discharge electrode must be replaced regularly, resulting in high maintenance costs.
[0013] 3. Laser absorption spectroscopy (TDLAS / CEAS), the principle of which is to monitor concentration changes in real time based on the absorption characteristics of gases to lasers of specific wavelengths. It mainly monitors H2 and O2 in argon (Ar) as a protective gas online (response time <100ms); and continuously monitors CO2 and H2O in synthetic air as a dilution gas. Its advantages are non-contact detection (no sampling required, direct penetration of pipelines or storage tanks), strong anti-interference (high selectivity (such as CO2's characteristic absorption in the 4.26μm band)), and its determination is limited by gas selectivity (the wavelength needs to be customized for the target gas (such as NH3 requires a 1572nm laser)), expensive equipment (the cost of a single system exceeds 500,000 yuan), and the inability to detect gases with overlapping spectra (such as CO and H2O in the near-infrared region).
[0014] 4. Electrochemical sensors: This method generates an electrical signal through a redox reaction between gas and electrodes. It primarily detects O2 and H2S in the shielding gas hydrogen (H2) (ppm level). It also provides online monitoring of O2 and CO in the diluent gas nitrogen (N2). Its advantages include low cost (sensor prices range from approximately 1,000 to 5,000 yuan) and real-time response (detection speed < 1 second). Its disadvantages include a short lifespan (sensors typically require replacement every 1 to 3 years), cross-interference (humidity and temperature fluctuations affect accuracy), and suitability only for reactive gases (such as O2 and H2S). It cannot detect inert impurities.
[0015] 5. MOFs (Metal Organic Framework) Sensors: The principle behind MOFs sensors is that they adsorb specific gases through pore selectivity and functional groups, triggering changes in conductivity or optical signals. They are primarily used for detecting VOCs (benzene and toluene) in helium (He) as a protective gas (ppb level) and for trace analysis of NH3 and H2O in nitrogen (N2) as a diluent gas. Their advantages include high selectivity (customizable pore size, such as a 0.4nm pore size for selective CO2 adsorption), room temperature operation (no heating or complex pretreatment required), and ppt-level detection accuracy. Their disadvantages include poor stability (performance degrades with long-term exposure to humidity or oxygen) and an inability to detect metal impurities in inert gases (such as He and Ne).
[0016] 6. Mass spectrometry (MS) is based on the principle of ionizing gases and separating them according to their mass-to-charge ratio, enabling simultaneous analysis of multiple components. It is primarily used to detect metallic impurities such as Fe and Cr in ultrapure argon (Ar) as a protective gas (ppb level) and to analyze trace organic pollutants (such as SF6) in synthetic air used as a dilution gas. Its advantages include ultra-high sensitivity (detection limit of 0.1 ppb, capable of identifying unknown impurities) and simultaneous multi-element detection (covering 20+ elements in a single analysis). Its disadvantages include expensive equipment (a complete system costs over 2 million yuan), complex operation (requiring professional expertise and high maintenance costs), and the need to convert the gas into plasma, making it incapable of directly analyzing inert gases.
[0017] 7. In situ infrared spectroscopy (FTIR) utilizes the absorption characteristics of infrared light to analyze the vibrational energy levels of gas molecules. It primarily monitors CO2 and CH4 in the shielding gas argon (Ar) and performs real-time analysis of H2O and NH3 in the diluent gas nitrogen (N2). Advantages include rapid scanning, a single analysis time of less than 1 minute, and non-destructive performance (samples can be recovered for repeated testing). Disadvantages include low sensitivity, typically at the ppm level (trace levels require enrichment), spectral interference (complex gas combinations can easily lead to overlapping absorption peaks), the need for regular calibration, and high maintenance costs.
[0018] The above-mentioned various trace impurity detection methods all have their own limitations and shortcomings, and cannot meet the requirements for efficient and high-precision detection of electronic mixed gases. Summary of the Invention
[0019] In view of the above-mentioned defects of the prior art, the purpose of the present invention is to provide a device and method for detecting trace impurities in electronic mixed gas, which can perform classified pre-detection and processing to ensure that the final detection result achieves high accuracy.
[0020] The objective of the present invention is achieved through such technical solution:
[0021] The device for detecting trace impurities in electronic mixed gas comprises:
[0022] The gas tank to be inspected contains the electronic mixed gas to be inspected;
[0023] The mass spectrometer is connected to the gas tank to be inspected through a mass spectrometer valve;
[0024] The metal impurity processing unit, the head end of which is connected to the gas tank to be inspected through the impurity removal valve and the first flow meter;
[0025] The dehumidification unit, the head end of which is connected to the metal impurity treatment unit through a dehumidification valve;
[0026] a gas chromatograph, which is connected to the tail end of the dehumidification unit through a chromatographic valve;
[0027] The multi-type and multi-stage MOFs sensor detection unit performs multi-stage combined detection according to the impurity type, and is connected to the tail end of the gas chromatograph through a detection valve;
[0028] The gas source supplement units are respectively connected to the multi-stage MOFs sensor detection units;
[0029] The multi-type and multi-level MOFs sensor detection unit includes:
[0030] an air inlet pump, the air inlet of which is connected to the air outlet of the gas chromatograph;
[0031] A receiving tank, wherein the opening is connected to the air outlet of the air intake pump;
[0032] Several groups of multi-stage MOFs sensor detection lines, each head end of which is connected to an opening of a storage tank through a second flow meter; the gas source replenishment unit is connected to each group of multi-stage MOFs sensor detection lines; the multi-stage MOFs sensor detection line includes at least two detection mechanisms connected in series; the storage tank is connected to adjacent detection mechanisms and between adjacent detection mechanisms in sequence through a constant pressure relief valve and a transfer valve; the gas outlet of the detection mechanism at the end of the multi-stage MOFs sensor detection line is provided with an exhaust valve;
[0033] The detection mechanism includes:
[0034] A detection tank containing a MOFs sensor;
[0035] A pressure gauge connected to the interior of the test tank;
[0036] A booster pump, the air inlet of which is connected to the air outlet of the air source replenishing unit;
[0037] A pressure and flow stabilizing valve, the air inlet of which is connected to the air outlet of the booster pump;
[0038] The stop valve has an air inlet connected to the air outlet of the pressure and flow stabilizing valve, and the air outlet is connected to the interior of the detection tank.
[0039] Furthermore, the metal impurity treatment unit includes an adsorption part and a recovery part; the adsorption part adsorbs metal impurities in the gas; the recovery part neutralizes the charge in the gas molecules discharged from the adsorption part;
[0040] The structure of the recovery part is the same as that of the adsorption part;
[0041] The adsorption part includes:
[0042] The adsorption tank, the head end is connected to the gas tank to be inspected through a debris removal valve, and the inner wall is insulated;
[0043] The flow equalizing component is installed at the head end of the adsorption tank, facing the impurity removal valve;
[0044] The charged component is arranged in the adsorption tank, facing the current balancing component and located downstream of the current balancing component; the surface of the charged component is conductive and is electrically connected to one pole of the power supply;
[0045] The adsorption component is arranged at the tail end of the adsorption tank, facing the charged component and located downstream of the charged component; the surface of the adsorption component is non-conductive and the interior is electrically connected to the other electrode of the power supply;
[0046] The recovery unit includes:
[0047] The recovery tank, whose head end is connected to the tail end of the adsorption tank through a recovery valve, neutralizes the charge of the gas molecules that have been charged after passing through the adsorption part; the tail end of the recovery tank is connected to the multi-type multi-level MOFs sensor detection unit;
[0048] The charge transfer component is arranged in the recovery tank; the surface of the charge transfer component is conductive and grounded.
[0049] Furthermore, the current balancing component includes:
[0050] A first flow balancing plate is perpendicular to the gas flow direction in the adsorption tank; first flow balancing holes are evenly arranged on the first flow balancing plate; the diameter of the first flow balancing holes does not exceed 5 mm; the total hole area of the first flow balancing holes of the first flow balancing plate is 30% to 40% of the plate area of the first flow balancing plate;
[0051] A second flow equalizing plate is located downstream of the first flow equalizing plate, perpendicular to the gas flow direction inside the adsorption tank, and is spaced from the first flow equalizing plate by a distance not less than 20 times the diameter of the first flow equalizing hole. The second flow equalizing hole is evenly arranged on the second flow equalizing plate. The diameter of the second flow equalizing hole does not exceed 2 mm. The total hole area of all the second flow equalizing holes on the second flow equalizing plate is 40% to 50% of the plate area of the second flow equalizing plate. The second flow equalizing hole is staggered with the first flow equalizing hole.
[0052] The third flow equalizing plate is perpendicular to the gas flow direction inside the adsorption tank, located downstream of the second flow equalizing plate, and the distance between the second flow equalizing plate and the second flow equalizing plate is not less than 10 times the diameter of the second flow equalizing hole; the third flow equalizing holes are evenly arranged on the third flow equalizing plate; the diameter of the third flow equalizing hole does not exceed 1 mm; the total hole area of all third flow equalizing holes on the third flow equalizing plate is 50% to 55% of the plate area of the third flow equalizing plate; the third flow equalizing hole is staggered with the second flow equalizing hole; the distance between the third flow equalizing plate and the charged component is not less than 10 times the diameter of the third flow equalizing hole.
[0053] Furthermore, the charged component includes a plurality of charged conductive sheets, which are evenly spaced and distributed in a dot-like manner along the transverse cross-section of the adsorption tank; the charged conductive sheets are divided into at least three layers and are arranged in sequence along the internal gas flow direction of the adsorption tank; the charged conductive sheets of each layer are electrically connected to each other, pass through the adsorption tank and are electrically connected to one pole of the power supply; adjacent charged conductive sheets are staggered along the internal gas flow direction of the adsorption tank;
[0054] The charged conductive sheet comprises:
[0055] Sheet, a long rectangular sheet;
[0056] The corner piece is in the shape of a triangular piece, with the bottom part fixed to one end of the piece;
[0057] The diverter cover is umbrella-shaped, with the tip fixed to the tip of the corner piece. The tip of the diverter cover faces the internal gas flow direction of the attached tank; the interval between adjacent charged conductive sheets is 2-3 times the diameter of the diverter cover; the sheet width is 0.3-0.5 times the diameter of the diverter cover, and the length is 5-10 times the diameter of the diverter cover.
[0058] Furthermore, the adsorption assembly includes a plurality of adsorption plates arranged at uniform intervals, the plate surfaces of the adsorption plates being parallel to the internal gas flow direction of the attached tank; the spacing between the adsorption plates being 0.8-1.2 times the diameter of the diverter hood; the adsorption plates being electrically connected to each other and electrically connected to the other pole of the power supply through the adsorption tank; and the surface of the adsorption assembly being coated with an insulating coating;
[0059] The structure of the charge transfer component is the same as that of the charged component and the adsorption component in the adsorption part.
[0060] Furthermore, a deflector is provided in the tail of the adsorption tank, the opening of which faces the adsorption assembly, and an opening is provided at the tail end, which is connected to the recovery valve; the adsorption part also includes a circulation pump and a circulation valve, the air inlet end is connected to the opening at the tail end of the adsorption tank through the circulation valve, and the air outlet end is connected to the head end of the adsorption tank; the circulation pump and the inner wall of its pipeline are coated with insulating material.
[0061] Furthermore, the source supplement unit includes:
[0062] The hydrogen tank is connected to the booster pump and the detection tank of each detection mechanism through the hydrogen valve;
[0063] The oxygen tank is connected to the booster pump and the detection tank of each detection mechanism through the oxygen valve.
[0064] Furthermore, the multi-type and multi-level MOFs sensor detection unit further includes a temperature stabilization mechanism;
[0065] Several circulating heat exchange components are respectively wrapped around the outer surfaces of the detection tank, hydrogen tank, and oxygen tank;
[0066] The energy storage tank is kept at a constant temperature through an external heat exchange system;
[0067] The heat exchange pump connects the energy storage tank with each circulating heat exchange component through a heat exchange valve.
[0068] Furthermore, the detection mechanism further includes:
[0069] A pressure equalizing plate, arranged upstream of the MOFs sensor, having a plurality of perforations on its surface;
[0070] The two ends of the suction booster pump are respectively connected to the head end and the tail end of the detection tank, and the connecting ports are respectively located upstream of the pressure equalizing plate and downstream of the MOFs sensor.
[0071] A method for detecting trace impurities in an electronic mixed gas comprises the following steps:
[0072] S1. Place the gas to be tested into the gas tank to be tested;
[0073] S2, close all valves and open the quality valve;
[0074] S3. After all the gas in the pipeline between the mass spectrometer and the gas tank to be tested is replaced by the gas to be tested, the mass spectrometer is turned on to detect the types of impurities in the gas to be tested. After the test is completed, the mass spectrometer valve is closed.
[0075] S4. Close the impurity removal valve and the mass flow valve, and open all other valves; connect the exhaust valve through the vacuum equipment to evacuate the metal impurity treatment unit, the dehumidification unit, and the multi-type multi-stage MOFs sensor detection unit; until the vacuum degree meets the requirements; close the vacuum equipment, then open the oxygen valve and the hydrogen valve, and after the injected hydrogen and oxygen reach a certain pressure, close the oxygen valve and the hydrogen valve after injection and connect the exhaust valve through the vacuum equipment, repeat the above operation several times to reduce the impurity gas in the detection system to a minimum;
[0076] S6. Close the dehumidification valve, open the impurity removal valve, and energize the adsorption unit. The metal impurities in the gas flowing into the adsorption tank are evenly distributed by the flow balancing component and then come into contact with the charged component, becoming charged. The metal impurities then move toward the adsorption component under the action of the airflow and are finally adsorbed on the surface of the adsorption component.
[0077] S7. When the pressure in the adsorption tank reaches a predetermined value, close the impurity removal valve; and read the flow data on the first flow meter;
[0078] S8. Turn on the circulation pump to allow the metal impurities in the gas in the adsorption tank to be adsorbed by the adsorption component as much as possible;
[0079] S9, the circulation pump is turned on for a certain period of time and then turned off, the charge transfer component in the recovery tank is energized, and then the recovery valve is opened;
[0080] S10, the gas with metal impurities removed enters the recovery tank to restore the charge balance;
[0081] S11, open the dehumidification valve, the gas enters the dehumidification unit, and absorbs the moisture in the air;
[0082] S12, opening the color valve, the gas enters the gas chromatograph, and the gas chromatograph detects the type and amount of gas in the gas;
[0083] S13, starting a corresponding number of groups of multi-stage MOFs sensor detection lines according to the number of impurity gas types detected by the gas chromatograph;
[0084] A MOFs sensor corresponding to each impurity type is placed in each group of multi-stage MOFs sensor detection lines;
[0085] S14, open the detection valve, start the air inlet pump, and compress the detection gas into the container;
[0086] S15. When the pressure in the container reaches a predetermined value, each group of multi-stage MOFs sensors is opened in turn to detect the content of each gas impurity. The specific detection steps are as follows:
[0087] SJ1: Open the constant pressure relief valve and transfer valve upstream of the first detection mechanism in each set of multi-stage MOFs sensor detection lines. The gas enters the detection tank after being decompressed and contacts the MOFs sensor inside the detection tank. The specific impurity gas to be detected is adsorbed by the MOFs sensor.
[0088] SJ2. Check the pressure inside the container using a pressure gauge. When the pressure inside the container reaches the control pressure of the constant pressure relief valve, close the transfer valve upstream of the first detection mechanism; read the data from the second flow meter.
[0089] SJ3. Start the suction pump to circulate the gas in the detection tank to the MOFs sensor, so that the MOFs sensor can absorb as much specific impurity gas as possible.
[0090] SJ4. After a certain period of time, read the MOFs sensor data in the first detection mechanism. If the data changes, it means that the MOFs sensor has detected the impurity gas; open the constant pressure relief valve and transfer valve upstream of the second detection mechanism detected by the multi-stage MOFs sensor detection line. At the same time, open the hydrogen valve or oxygen valve corresponding to the supplementary gas source, start the booster pump, open the pressure and flow stabilizing valve and the shut-off valve; the supplementary gas source is hydrogen or oxygen with a molecular weight close to that of the gas molecules detected by the multi-stage MOFs sensor detection line;
[0091] SJ5. After the pressure in the container of the second detection mechanism reaches the control pressure of the constant pressure relief valve upstream of the first detection mechanism, close the hydrogen valve or oxygen valve, the booster pump, the pressure and flow stabilizing valve, and the shut-off valve;
[0092] SJ6. After a period of time, the MOFs sensor data in the second detection mechanism is read. If the data changes, it means that the MOFs sensor has detected the impurity gas;
[0093] SJ7. Then, according to steps SJ3 to SJ5, gas is injected into each detection mechanism in the group of multi-stage MOFs sensor detection lines until the MOFs sensor data in the detection mechanism injected with gas does not change;
[0094] SJ8. Summarize the data of each MOFs sensor in the group of multi-stage MOFs sensor detection lines, determine the total amount of adsorbed specific impurity gas after calculation, and then calculate the content of the specific impurity gas based on the total amount of gas measured by the second flow meter on each group of multi-stage MOFs sensor detection lines.
[0095] Due to the adoption of the above technical solution, the present invention has the following advantages:
[0096] 1. Combining multiple cutting-edge impurity gases according to actual needs, we can achieve detection accuracy that exceeds any single existing detection method based on existing detection technology. A single impurity gas can be detected at the ppb level. At the same time, the detection process is less affected by the detection interference, that is, MOFs detection is performed separately for specific impurity gas types.
[0097] 2. The system organically integrates multiple impurity detection technologies, effectively pre-processes each impurity before testing, reduces the interference of other impurities on the impurity types that need to be detected, and improves the accuracy and sensitivity of detection.
[0098] 3. Multi-level MOFs are used to detect each gas impurity. Compared with conventional MOFs detection, all impurity gases that are free in the container space and not adsorbed by MOFs can be adsorbed, thereby improving the positive error of the detection and avoiding damage to the wafer caused by negative error detection results.
[0099] 4. The setting of the dehumidification unit can reduce the entry of water vapor into the MOFs sensor and increase the service life of the MOFs sensor.
[0100] 5. The booster pump and pressure and flow stabilizing valve can keep the pressure of the detection mechanism relatively stable, and can also reduce the impact of high-speed airflow on MOFs when the supplementary gas flows into the detection mechanism, so that the specific impurity gas adsorbed in the MOFs will not be separated as much as possible.
[0101] Other advantages, objects and features of the present invention will be described in part in the following description and, in part, will be apparent to those skilled in the art based on an examination of the following or may be learned from the practice of the invention. BRIEF DESCRIPTION OF THE DRAWINGS
[0102] Figure 1 1 is a simplified structural diagram of the device for detecting trace impurities in an electronic mixed gas in this embodiment;
[0103] Figure 2 is a schematic structural diagram of the metal impurity processing unit in this embodiment;
[0104] Figure 3 is a schematic cross-sectional structural diagram of the metal impurity processing unit in this embodiment;
[0105] Figure 4 yes Figure 3 A in the middle is an enlarged structural diagram;
[0106] Figure 5Schematic diagram of the plan view structure with conductive sheet in this embodiment;
[0107] Figure 6 Schematic diagram of the structure of the multi-type multi-stage MOFs sensor detection unit and the gas source supplement unit in this embodiment;
[0108] Figure 7 It is a structural cross-sectional view of a single detection mechanism in this embodiment.
[0109] In the figure: 1. Gas tank to be inspected; 2. Mass spectrometer; 3. Metal impurity treatment unit; 31. Adsorption unit; 311. Adsorption tank; 3111. Flow guide cover; 3121. First flow equalizing plate; 3122. Second flow equalizing plate; 3123. Third flow equalizing plate; 313. Charged component; 31311. Sheet; 31312. Corner piece; 31313. Flow divider; 3141. Adsorption plate; 32. Recovery unit; 321. Recovery tank; 322. Charge transfer component; 33. Circulation pump; 4. Dehumidification unit; 5. Multiple types of multi-stage MOFs sensor detection unit; 51. Air intake pump; 52. Storage tank; 53. Multi-stage MOFs sensor detection line; 531. Detection tank; 532. Air pressure Table; 533. Booster pump; 534. Pressure and flow stabilizing valve; 535. Stop valve; 536. MOFs sensor; 54. Constant pressure relief valve; 55. Transfer valve; 56. Exhaust valve; 571. Circulating heat exchange component; 572. Energy storage tank; 573. External heat exchange system; 574. Heat exchange pump; 58. Pressure equalizing plate; 59. Suction pump; 6. Gas source replenishment unit; 61. Hydrogen tank; 62. Hydrogen valve; 63. Oxygen tank; 64. Oxygen valve; 71. Mass Spectrometer valve; 72. Impurity removal valve; 73. Dehumidification valve; 74. Detection valve; 75. Recovery valve, 76. Circulation valve; 77. Chromatographic valve; 78. Heat exchange valve; 81. First flow meter; 82. Second flow meter; 9. Gas chromatograph.
[0110] The present invention will be further described below with reference to the embodiments. Example
[0111] like Figure 1-7 As shown, the device for detecting trace impurities in electronic mixed gas includes:
[0112] The gas tank to be tested 1 contains the electronic mixed gas to be tested;
[0113] The mass spectrometer 2 is connected to the gas tank 1 to be inspected via the mass spectrometer valve 71;
[0114] The head end of the metal impurity treatment unit 3 is connected to the gas tank 1 to be inspected through the impurity removal valve 72 and the first flow meter 81;
[0115] The dehumidification unit 4, the head end of which is connected to the metal impurity treatment unit 3 through the dehumidification valve 73;
[0116] a gas chromatograph 9, which is connected to the tail end of the dehumidification unit 4 via a chromatographic valve 77;
[0117] The multi-type and multi-stage MOFs sensor detection unit 5 performs multi-stage combined detection according to the impurity type, and is connected to the tail end of the gas chromatograph 9 through the detection valve 74;
[0118] The gas source supplement unit 6 is respectively connected to the detection unit of the multi-stage MOFs sensor 536;
[0119] The multi-type multi-level MOFs sensor detection unit 5 includes:
[0120] An air inlet pump 51, the air inlet of which is connected to the air outlet of the gas chromatograph 9;
[0121] The accommodating tank 52 has an opening connected to the air outlet of the air inlet pump 51;
[0122] Several groups of multi-stage MOFs sensor detection lines 53 are connected at their head ends to the openings of the storage tank 52 through second flow meters 82. The air source replenishment unit 6 is connected to each group of multi-stage MOFs sensor detection lines 53. The multi-stage MOFs sensor detection lines 53 include at least two detection mechanisms connected in series. The storage tank 52 is connected to adjacent detection mechanisms, and to detection mechanisms between adjacent detection mechanisms, in sequence, through constant pressure relief valves 54 and transfer valves 55. The gas outlet of the detection mechanism at the end of the multi-stage MOFs sensor detection line 53 is provided with an exhaust valve 56.
[0123] The detection mechanism includes:
[0124] A detection tank 531 , housing a MOFs sensor 536;
[0125] The pressure gauge 532 is connected to the interior of the detection tank 531;
[0126] The booster pump 533 has an air inlet connected to the air outlet of the air source replenishing unit 6;
[0127] The pressure and flow stabilizing valve 534 has an air inlet connected to the air outlet of the booster pump 533;
[0128] The shut-off valve 535 has an air inlet connected to the air outlet of the pressure and flow stabilizing valve 534 , and an air outlet connected to the interior of the detection tank 531 .
[0129] By combining multiple cutting-edge impurity gases based on actual needs, we can achieve detection accuracy that exceeds any single existing detection method based on existing detection technology. Single impurity gases can be detected at the ppb level, and some impurity gases can be detected at the double-digit ppb level, and some impurity gases can even be detected at the single-digit ppb level. At the same time, the detection process is less subject to detection interference, that is, MOFs detection is performed separately for specific impurity gas types. By organically integrating multiple impurity detection technologies, each impurity is effectively pretreated before detection, reducing the interference of other impurities on the impurity types to be detected and improving the accuracy and sensitivity of detection. Multi-level MOFs detection is performed on each gas impurity. Compared with conventional MOFs detection, all impurity gases that are free in the container space and not adsorbed by the MOFs can be adsorbed, thereby improving the positive error of the detection and avoiding damage to the wafer caused by negative error detection results.
[0130] The boost pump 533 and the pressure and flow stabilizing valve 534 are provided so that the pressure of the detection mechanism can be kept relatively stable, and the impact of the high-speed airflow formed when the supplementary gas flows into the detection mechanism on the MOFs can be reduced, so that the specific impurity gas adsorbed in the MOFs is prevented from escaping as much as possible.
[0131] In this example, the metal impurity treatment unit 3 includes an adsorption portion 31 and a recovery portion 32; the adsorption portion 31 adsorbs metal impurities in the gas; the recovery portion 32 neutralizes the charge in the gas molecules discharged from the adsorption portion 31;
[0132] The structure of the recovery part 32 is the same as that of the adsorption part 31;
[0133] The adsorption unit 31 includes:
[0134] The adsorption tank 311, the head end of which is connected to the gas tank 1 to be inspected through the impurity removal valve 72, and the inner wall is insulated;
[0135] The flow balancing component is provided at the head end of the adsorption tank 311 and directly faces the impurity removal valve 72;
[0136] The charged component 313 is disposed in the adsorption tank 311, facing the current balancing component and located downstream of the current balancing component; the surface of the charged component 313 is conductive and electrically connected to one pole of the power supply;
[0137] The adsorption component is arranged at the tail end of the adsorption tank 311, facing the charged component 313, and located downstream of the charged component 313; the surface of the adsorption component is non-conductive, and the interior is electrically connected to the other electrode of the power supply;
[0138] The recovery unit 32 includes:
[0139] The recovery tank 321 has its head end connected to the tail end of the adsorption tank 311 through the recovery valve 75 to neutralize the charge of the gas molecules that have been charged after passing through the adsorption part 31; the tail end of the recovery tank 321 is connected to the multi-type multi-stage MOFs sensor detection unit 5;
[0140] The charge transfer component 322 is disposed in the recovery tank 321 ; the surface of the charge transfer component 322 is conductive and grounded.
[0141] The metal impurities are separated by charge adsorption, thereby reducing the metal impurities from entering the multi-stage MOFs sensor detection line 53 and combining with MOFs, resulting in inaccurate detection by the MOFs sensor 536.
[0142] In this embodiment, the current balancing component includes:
[0143] The first flow balancing plate 3121 is perpendicular to the gas flow direction in the adsorption tank 311 ; the first flow balancing holes are evenly distributed on the first flow balancing plate 3121 ; the diameter of the first flow balancing holes does not exceed 5 mm; the total hole area of the first flow balancing holes of the first flow balancing plate 3121 is 30% to 40% of the plate area of the first flow balancing plate 3121 ;
[0144] The second equalizing plate 3122 is perpendicular to the gas flow direction within the adsorption tank 311 and is located downstream of the first equalizing plate 3121. The distance between the second equalizing plate 3121 and the first equalizing plate 3121 is no less than 20 times the diameter of the first equalizing holes. The second equalizing holes are evenly distributed on the second equalizing plate 3122. The diameter of the second equalizing holes does not exceed 2 mm. The total hole area of all the second equalizing holes on the second equalizing plate 3122 is 40% to 50% of the plate area of the second equalizing plate 3122. The second equalizing holes are staggered with the first equalizing holes.
[0145] The third flow equalizing plate 3123 is perpendicular to the internal gas flow direction of the adsorption tank 311, is located downstream of the second flow equalizing plate 3122, and is spaced apart from the second flow equalizing plate 3122 by no less than 10 times the diameter of the second flow equalizing hole; the third flow equalizing holes are evenly arranged on the third flow equalizing plate 3123; the diameter of the third flow equalizing hole does not exceed 1 mm; the total hole area of all third flow equalizing holes on the third flow equalizing plate 3123 is 50% to 55% of the plate area of the third flow equalizing plate 3123; the third flow equalizing hole is staggered with the second flow equalizing hole; the distance between the third flow equalizing plate 3123 and the charged component 313 is no less than 10 times the diameter of the third flow equalizing hole.
[0146] The flow equalizing plate can make the gas flow through the charged component 313 as much as possible, ensuring that the metal impurities in the gas can be fully adsorbed.
[0147] In this embodiment, the charged component 313 includes a plurality of charged conductive sheets, which are evenly spaced and distributed in a dot-like manner along the transverse cross-section of the adsorption tank 311. The charged conductive sheets are divided into at least three layers and are arranged in sequence along the internal gas flow direction of the adsorption tank 311. The charged conductive sheets of each layer are electrically connected to each other, pass through the adsorption tank 311, and are electrically connected to one pole of the power supply. Adjacent charged conductive sheets are staggered along the internal gas flow direction of the adsorption tank.
[0148] The charged conductive sheet comprises:
[0149] Sheet 31311 is in the form of a long rectangular sheet;
[0150] Corner piece 31312 is in the shape of a triangular piece, the bottom of which is fixedly connected to one end of piece 31311;
[0151] The diverter hood 31313 is umbrella-shaped, with its tip fixed to the tip of the corner piece 31312. The tip of the diverter hood 31313 faces the internal gas flow direction of the attached tank; the interval between adjacent charged conductive sheets is 2-3 times the diameter of the diverter hood 31313; the width of the sheet 31311 is 0.3-0.5 times the diameter of the diverter hood 31313, and the length is 5-10 times the diameter of the diverter hood 31313.
[0152] The above design can not only ensure that metal impurities can be fully adsorbed, but also greatly improve the adsorption efficiency.
[0153] In this embodiment, the adsorption assembly includes a plurality of evenly spaced adsorption plates 3141, with the surface direction of the adsorption plates 3141 parallel to the internal gas flow direction of the attached tank; the spacing between the adsorption plates 3141 is 0.8-1.2 times the diameter of the diverter cover 31313; the adsorption plates 3141 are electrically connected to each other and pass through the adsorption tank 311 to be electrically connected to the other pole of the power supply; the surface of the adsorption assembly is coated with an insulating coating;
[0154] The structure of the charge transfer component 322 is the same as that of the charged component 313 and the adsorption component in the adsorption part 31 .
[0155] In this embodiment, a deflector 3111 is provided in the tail of the adsorption tank 311, the opening of which faces the adsorption assembly, and an opening is provided at the tail end, which is connected to the recovery valve 75; the adsorption part 31 also includes a circulation pump 33 and a circulation valve 76, the air inlet end is connected to the opening at the tail end of the adsorption tank 311 through the circulation valve 76, and the air outlet end is connected to the head end of the adsorption tank 311; the circulation pump 33 and the inner wall of its pipeline are coated with insulating material.
[0156] The gas can be circulated to contact the charged component 313 through the circulation pump 33 to ensure that the metal impurities are adsorbed as much as possible.
[0157] In this embodiment, the source supplement unit includes:
[0158] The hydrogen tank 61 is connected to the booster pump 533 of each detection mechanism and the detection tank 531 through the hydrogen valve 62;
[0159] The oxygen tank 63 is connected to the booster pump 533 and the detection tank 531 of each detection mechanism through the oxygen valve 64.
[0160] Hydrogen and oxygen do not react with the active gases or impurities in the shielding and diluent gases. The purity and concentration of hydrogen and oxygen produced by water electrolysis can reach over 99%. Impurities in either oxygen or hydrogen alone are limited to the other gas (hydrogen or oxygen), preventing the introduction of other impurities. Furthermore, when used alone, the concentrations of either gas do not reach explosion or combustion limits, making them extremely safe.
[0161] In this embodiment, the multi-type multi-level MOFs sensor detection unit 5 further includes a temperature stabilization mechanism;
[0162] Several circulating heat exchange components 571 are respectively wrapped around the outer surfaces of the detection tank 531, the hydrogen tank 61, and the oxygen tank 63;
[0163] The energy storage tank 572 is maintained at a constant temperature by an external heat exchange system 573;
[0164] The heat exchange pump 574 connects the energy storage tank 572 with each circulating heat exchange component 571 through the heat exchange valve 78.
[0165] After a MOF sensor 536 in a detection mechanism absorbs a specific impurity gas and then injects its associated gas into the next detection mechanism, a temperature stabilization mechanism is incorporated to minimize the escape of the specific impurity gas from the MOFs and its entry into the next detection mechanism. This design, based on the booster pump 533, maintains both consistent pressure and temperature, ensuring stable and consistent adsorption of specific impurity gases by the MOFs in each detection mechanism, further improving detection accuracy and sensitivity.
[0166] At the same time, while controlling temperature and pressure, hydrogen and oxygen are used as supplemental gases to reduce desorption from MOFs. The closer the molecular weight of the supplemental gas injected into the detection mechanism is to that of the absorbed specific impurity gas, the less likely that specific impurity gas will escape from the MOFs. Therefore, hydrogen or oxygen can be selected as the supplemental gas based on actual conditions.
[0167] In this embodiment, the detection mechanism further includes:
[0168] The pressure equalizing plate 58 is provided upstream of the MOFs sensor 536 and has a plurality of perforations on its surface;
[0169] The two ends of the suction booster pump 59 are connected to the head end and the tail end of the detection tank 531 respectively, and the connecting ports are located upstream of the pressure equalizing plate 58 and downstream of the MOFs sensor 536 respectively.
[0170] The suction booster pump 59 can cause the gas to circulate through the MOFs multiple times, so that specific impurity gases in the gas can be adsorbed as much as possible.
[0171] A method for detecting trace impurities in an electronic mixed gas comprises the following steps:
[0172] S1, placing the gas to be tested into the gas tank 1 to be tested;
[0173] S2, close all valves and open the mass valve 71;
[0174] S3, until the gas in the pipeline between the mass spectrometer 2 and the gas tank 1 to be inspected is completely replaced by the gas to be inspected; open the mass spectrometer 2 to detect the types of impurities in the gas to be inspected; after the detection is completed, close the mass spectrometer valve 71;
[0175] S4, close the impurity removal valve 72 and the mass flow valve 71, and open all other valves; connect the exhaust valve 56 through the vacuum equipment, and evacuate the metal impurity treatment unit 3, the dehumidification unit 4, and the multi-type multi-level MOFs sensor detection unit 5; until the vacuum degree meets the requirements; close the vacuum equipment, then open the oxygen valve 64 and the hydrogen valve 62, and after the injected hydrogen and oxygen reach a certain pressure, close the oxygen valve 64 and the hydrogen valve 62 after injection, connect the exhaust valve through the vacuum equipment, and repeat the above operation several times to reduce the impurity gas in the detection system to a minimum;
[0176] S6. Close the dehumidification valve 73, open the impurity removal valve 72, and energize the adsorption unit 31. The metal impurities in the gas flowing into the adsorption tank 311 are evenly distributed by the flow balancing component and then contact the charged component 313, becoming charged. The metal impurities then move toward the adsorption component under the action of the airflow and are finally adsorbed on the surface of the adsorption component.
[0177] S7. When the pressure in the adsorption tank 311 reaches a predetermined value, the impurity removal valve 72 is closed; and the flow rate data on the first flow meter 81 is read;
[0178] S8. Turn on the circulation pump 33 so that the metal impurities in the gas in the adsorption tank 311 are adsorbed by the adsorption assembly as much as possible;
[0179] S9, the circulation pump 33 is turned on for a certain period of time and then turned off, the charge transfer component 322 in the recovery tank 321 is energized, and then the recovery valve 75 is opened;
[0180] S10, the gas with metal impurities removed enters the recovery tank 321 to restore the charge balance;
[0181] S11, open the dehumidification valve 73, the gas enters the dehumidification unit 4, and absorbs the moisture in the gas;
[0182] S12, open the color valve, the gas enters the gas chromatograph, and the gas chromatograph 9 detects the type and amount of gas in the gas;
[0183] S13, starting a corresponding number of groups of multi-stage MOFs sensor detection lines 53 according to the number of impurity gas types detected by the gas chromatograph 9;
[0184] A MOFs sensor 536 corresponding to each impurity type is placed in each group of multi-stage MOFs sensor detection lines 53;
[0185] S14, open the detection valve 74, start the air pump 51, and compress the detection gas into the container 52;
[0186] S15. When the pressure in the container 52 reaches a predetermined value, each group of multi-stage MOFs sensors 536 is opened in sequence to detect the content of each gas impurity. The specific detection steps are as follows:
[0187] SJ1. Open the constant pressure relief valve 54 and transfer valve 55 upstream of the first detection mechanism in each set of multi-stage MOFs sensor detection lines 53. After the gas is depressurized, it enters the detection tank 531 and contacts the MOFs sensor 536 in the detection tank 531. The specific impurity gas to be detected is adsorbed by the MOFs sensor 536.
[0188] SJ2. Check the pressure in the container 52 using the pressure gauge. When the pressure in the container 52 reaches the control pressure of the constant pressure relief valve 54, close the transfer valve 55 upstream of the first detection mechanism; read the data from the second flow meter 82.
[0189] SJ3. Start the suction pump 59 to circulate the gas in the detection tank 531 toward the MOFs sensor 536, so that the MOFs sensor 536 can absorb as much specific impurity gas as possible.
[0190] SJ4. After a certain period of time, the data of the MOFs sensor 536 in the first detection mechanism is read. If the data changes, it means that the MOFs sensor 536 has detected the impurity gas. The constant pressure relief valve 54 and the transfer valve 55 upstream of the second detection mechanism detected by the multi-stage MOFs sensor detection line 53 are opened. At the same time, the hydrogen valve 62 or oxygen valve 64 corresponding to the supplementary gas source is opened, the booster pump 533 is started, and the pressure and flow stabilizing valve 534 and the stop valve 535 are opened. The supplementary gas source is hydrogen or oxygen with a molecular weight close to that of the gas detected by the multi-stage MOFs sensor detection line 53.
[0191] SJ5. After the pressure in the storage tank 52 of the second detection mechanism reaches the control pressure of the constant pressure relief valve 54 upstream of the first detection mechanism, close the hydrogen valve 62 or the oxygen valve 64, the booster pump 533, the pressure and flow stabilizing valve 534, and the stop valve 535.
[0192] SJ6. After a period of time, the data of the MOFs sensor 536 in the second detection mechanism is read. If the data changes, it means that the MOFs sensor 536 has detected the impurity gas;
[0193] SJ7. Then, according to steps SJ3 to SJ5, gas is injected into each detection mechanism in the group of multi-stage MOFs sensor detection lines 53 until the data of the MOFs sensor 536 in the detection mechanism injected with gas does not change;
[0194] SJ8. Summarize the data of each MOFs sensor 536 in the group of multi-stage MOFs sensor detection lines 53, determine the total amount of adsorbed specific impurity gas after calculation, and then calculate the content of the specific impurity gas based on the total amount of gas in the second flow meter 82 on each group of multi-stage MOFs sensor detection lines 53.
[0195] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not limiting. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention can be modified or replaced by equivalents without departing from the purpose and scope of the technical solutions, which should all be included in the scope of the claims of the present invention.
Claims
1. A device for detecting trace impurities in electronic mixed gas, characterized in that: include: The gas tank to be inspected contains the electronic mixed gas to be inspected; The mass spectrometer is connected to the gas tank to be inspected through a mass spectrometer valve; The metal impurity processing unit, the head end of which is connected to the gas tank to be inspected through the impurity removal valve and the first flow meter; The dehumidification unit, the head end of which is connected to the metal impurity treatment unit through a dehumidification valve; a gas chromatograph, which is connected to the tail end of the dehumidification unit through a chromatographic valve; The multi-type and multi-stage MOFs sensor detection unit performs multi-stage combined detection according to the impurity type, and is connected to the tail end of the gas chromatograph through a detection valve; The gas source supplement units are respectively connected to the multi-stage MOFs sensor detection units; The multi-type and multi-level MOFs sensor detection unit includes: an air inlet pump, the air inlet of which is connected to the air outlet of the gas chromatograph; A receiving tank, wherein the opening is connected to the air outlet of the air intake pump; Several groups of multi-stage MOFs sensor detection lines, each head end of which is connected to an opening of a storage tank through a second flow meter; the gas source replenishment unit is connected to each group of multi-stage MOFs sensor detection lines; the multi-stage MOFs sensor detection line includes at least two detection mechanisms connected in series; the storage tank is connected to adjacent detection mechanisms and between adjacent detection mechanisms in sequence through a constant pressure relief valve and a transfer valve; the gas outlet of the detection mechanism at the end of each group of multi-stage MOFs sensor detection lines is provided with an exhaust valve; The detection mechanism includes: A detection tank containing a MOFs sensor; A pressure gauge connected to the interior of the test tank; A booster pump, the air inlet of which is connected to the air outlet of the air source replenishing unit; A pressure and flow stabilizing valve, the air inlet of which is connected to the air outlet of the booster pump; The stop valve has an air inlet connected to the air outlet of the pressure and flow stabilizing valve, and the air outlet is connected to the interior of the detection tank.
2. The device for detecting trace impurities in electronic mixed gas according to claim 1, characterized in that: The metal impurity treatment unit includes an adsorption part and a recovery part; the adsorption part adsorbs metal impurities in the gas; the recovery part neutralizes the charge in the gas molecules discharged from the adsorption part; The structure of the recovery part is the same as that of the adsorption part; The adsorption part includes: The adsorption tank, the head end is connected to the gas tank to be inspected through a debris removal valve, and the inner wall is insulated; The flow equalizing component is installed at the head end of the adsorption tank, facing the impurity removal valve; The charged component is arranged in the adsorption tank, facing the current balancing component and located downstream of the current balancing component; the surface of the charged component is conductive and is electrically connected to one pole of the power supply; The adsorption component is arranged at the tail end of the adsorption tank, facing the charged component and located downstream of the charged component; the surface of the adsorption component is non-conductive and the interior is electrically connected to the other electrode of the power supply; The recovery unit includes: The recovery tank, whose head end is connected to the tail end of the adsorption tank through a recovery valve, neutralizes the charge of the gas molecules that have been charged after passing through the adsorption part; the tail end of the recovery tank is connected to the multi-type multi-level MOFs sensor detection unit; The charge transfer component is arranged in the recovery tank; the surface of the charge transfer component is conductive and grounded.
3. The device for detecting trace impurities in electronic mixed gas according to claim 2, characterized in that: The current sharing component includes: A first flow balancing plate is perpendicular to the gas flow direction in the adsorption tank; first flow balancing holes are evenly arranged on the first flow balancing plate; the diameter of the first flow balancing holes does not exceed 5 mm; the total hole area of the first flow balancing holes of the first flow balancing plate is 30% to 40% of the plate area of the first flow balancing plate; A second flow equalizing plate is located downstream of the first flow equalizing plate, perpendicular to the gas flow direction inside the adsorption tank, and is spaced from the first flow equalizing plate by a distance not less than 20 times the diameter of the first flow equalizing hole. The second flow equalizing hole is evenly arranged on the second flow equalizing plate. The diameter of the second flow equalizing hole does not exceed 2 mm. The total hole area of all the second flow equalizing holes on the second flow equalizing plate is 40% to 50% of the plate area of the second flow equalizing plate. The second flow equalizing hole is staggered with the first flow equalizing hole. The third flow equalizing plate is perpendicular to the gas flow direction inside the adsorption tank, located downstream of the second flow equalizing plate, and the distance between the second flow equalizing plate and the second flow equalizing plate is not less than 10 times the diameter of the second flow equalizing hole; the third flow equalizing holes are evenly arranged on the third flow equalizing plate; the diameter of the third flow equalizing hole does not exceed 1 mm; the total hole area of all third flow equalizing holes on the third flow equalizing plate is 50% to 55% of the plate area of the third flow equalizing plate; the third flow equalizing hole is staggered with the second flow equalizing hole; the distance between the third flow equalizing plate and the charged component is not less than 10 times the diameter of the third flow equalizing hole.
4. The device for detecting trace impurities in electronic mixed gas according to claim 3, characterized in that: The charged assembly includes a plurality of charged conductive sheets, which are evenly spaced and distributed in a dot-like manner along the transverse cross-section of the adsorption tank. The charged conductive sheets are divided into at least three layers and are arranged in sequence along the internal gas flow direction of the adsorption tank. The charged conductive sheets of each layer are electrically connected to each other and pass through the adsorption tank to be electrically connected to one pole of the power supply. Adjacent charged conductive sheets are staggered along the internal gas flow direction of the adsorption tank. The charged conductive sheet comprises: Sheet, a long rectangular sheet; The corner piece is in the shape of a triangular piece, with the bottom part fixed to one end of the piece; The diverter cover is umbrella-shaped, with the tip fixed to the tip of the corner piece. The tip of the diverter cover faces the internal gas flow direction of the attached tank; the interval between adjacent charged conductive sheets is 2-3 times the diameter of the diverter cover; the sheet width is 0.3-0.5 times the diameter of the diverter cover, and the length is 5-10 times the diameter of the diverter cover.
5. The device for detecting trace impurities in electronic mixed gas according to claim 4, characterized in that: The adsorption assembly includes a plurality of evenly spaced adsorption plates, the surface direction of the adsorption plates being parallel to the internal gas flow direction of the attached tank; the spacing between the adsorption plates is 0.8-1.2 times the diameter of the diverter hood; the adsorption plates are electrically connected to each other and electrically connected to the other pole of the power supply through the adsorption tank; the surface of the adsorption assembly is coated with an insulating coating; The structure of the charge transfer component is the same as that of the charged component and the adsorption component in the adsorption part.
6. The device for detecting trace impurities in electronic mixed gas according to claim 5, characterized in that: A deflector is provided in the tail of the adsorption tank, with an opening facing the adsorption assembly, and an opening is provided at the tail end, which is connected to the recovery valve; the adsorption part also includes a circulation pump and a circulation valve, the air inlet end is connected to the opening at the tail end of the adsorption tank through the circulation valve, and the air outlet end is connected to the head end of the adsorption tank; the circulation pump and the inner wall of its pipeline are coated with insulating material.
7. The device for detecting trace impurities in electronic mixed gas according to claim 6, characterized in that: The source supplement unit includes: The hydrogen tank is connected to the booster pump and the detection tank of each detection mechanism through the hydrogen valve; The oxygen tank is connected to the booster pump and the detection tank of each detection mechanism through the oxygen valve.
8. The device for detecting trace impurities in electronic mixed gas according to claim 7, characterized in that: The multi-type and multi-level MOFs sensor detection unit also includes a temperature stabilization mechanism; Several circulating heat exchange components are respectively wrapped around the outer surfaces of the detection tank, hydrogen tank, and oxygen tank; The energy storage tank is kept at a constant temperature through an external heat exchange system; The heat exchange pump connects the energy storage tank with each circulating heat exchange component through a heat exchange valve.
9. The device for detecting trace impurities in electronic mixed gas according to claim 8, characterized in that: The detection mechanism also includes: A pressure equalizing plate, arranged upstream of the MOFs sensor, having a plurality of perforations on its surface; The two ends of the suction booster pump are respectively connected to the head end and the tail end of the detection tank, and the connecting ports are respectively located upstream of the pressure equalizing plate and downstream of the MOFs sensor.
10. The detection method of the device for detecting trace impurities in electronic mixed gas according to claim 9, characterized in that: The following steps are involved: S1. Place the gas to be tested into the gas tank to be tested; S2, close all valves and open the quality valve; S3. After all the gas in the pipeline between the mass spectrometer and the gas tank to be tested is replaced by the gas to be tested, the mass spectrometer is turned on to detect the types of impurities in the gas to be tested. After the test is completed, the mass spectrometer valve is closed. S4. Close the impurity removal valve and the mass flow valve, and open all other valves; connect the exhaust valve through the vacuum equipment to evacuate the metal impurity treatment unit, the dehumidification unit, and the multi-type multi-stage MOFs sensor detection unit; until the vacuum degree meets the requirements; close the vacuum equipment, then open the oxygen valve and the hydrogen valve, and after the injected hydrogen and oxygen reach a certain pressure, close the oxygen valve and the hydrogen valve after injection and connect the exhaust valve through the vacuum equipment, repeat the above operation several times to reduce the impurity gas in the detection system to a minimum; S6. Close the dehumidification valve, open the impurity removal valve, and energize the adsorption unit. The metal impurities in the gas flowing into the adsorption tank are evenly distributed by the flow balancing component and then come into contact with the charged component, becoming charged. The metal impurities then move toward the adsorption component under the action of the airflow and are finally adsorbed on the surface of the adsorption component. S7. When the pressure in the adsorption tank reaches a predetermined value, close the impurity removal valve; and read the flow data on the first flow meter; S8. Turn on the circulation pump to allow the metal impurities in the gas in the adsorption tank to be adsorbed by the adsorption component as much as possible; S9, the circulation pump is turned on for a certain period of time and then turned off, the charge transfer component in the recovery tank is energized, and then the recovery valve is opened; S10, the gas with metal impurities removed enters the recovery tank to restore the charge balance; S11, open the dehumidification valve, the gas enters the dehumidification unit, and absorbs the moisture in the air; S12, opening the color valve, the gas enters the gas chromatograph, and the gas chromatograph detects the type and amount of gas in the gas; S13, starting a corresponding number of groups of multi-stage MOFs sensor detection lines according to the number of impurity gas types detected by the gas chromatograph; A MOFs sensor corresponding to each impurity type is placed in each group of multi-stage MOFs sensor detection lines; S14, open the detection valve, start the air inlet pump, and compress the detection gas into the container; S15. When the pressure in the container reaches a predetermined value, each group of multi-stage MOFs sensors is opened in turn to detect the content of each gas impurity. The specific detection steps are as follows: SJ1: Open the constant pressure relief valve and transfer valve upstream of the first detection mechanism in each set of multi-stage MOFs sensor detection lines. The gas enters the detection tank after being decompressed and contacts the MOFs sensor inside the detection tank. The specific impurity gas to be detected is adsorbed by the MOFs sensor. SJ2. Check the pressure inside the container using a pressure gauge. When the pressure inside the container reaches the control pressure of the constant pressure relief valve, close the transfer valve upstream of the first detection mechanism; read the data from the second flow meter. SJ3. Start the suction pump to circulate the gas in the detection tank to the MOFs sensor, so that the MOFs sensor can absorb as much specific impurity gas as possible. SJ4. After a certain period of time, read the MOFs sensor data in the first detection mechanism. If the data changes, it means that the MOFs sensor has detected the impurity gas; open the constant pressure relief valve and transfer valve upstream of the second detection mechanism detected by the multi-stage MOFs sensor detection line. At the same time, open the hydrogen valve or oxygen valve corresponding to the supplementary gas source, start the booster pump, open the pressure and flow stabilizing valve and the shut-off valve; the supplementary gas source is hydrogen or oxygen with a molecular weight close to that of the gas molecules detected by the multi-stage MOFs sensor detection line; SJ5. After the pressure in the container of the second detection mechanism reaches the control pressure of the constant pressure relief valve upstream of the first detection mechanism, close the hydrogen valve or oxygen valve, the booster pump, the pressure and flow stabilizing valve, and the shut-off valve; SJ6. After a period of time, the MOFs sensor data in the second detection mechanism is read. If the data changes, it means that the MOFs sensor has detected the impurity gas; SJ7. Then, according to steps SJ3 to SJ5, gas is injected into each detection mechanism in the group of multi-stage MOFs sensor detection lines until the MOFs sensor data in the detection mechanism injected with gas does not change; SJ8. Summarize the data of each MOFs sensor in the group of multi-stage MOFs sensor detection lines, determine the total amount of adsorbed specific impurity gas after calculation, and then calculate the content of the specific impurity gas based on the total amount of gas measured by the second flow meter on each group of multi-stage MOFs sensor detection lines.