High-purity gas sampling method and device

Abstract

The invention relates to the field of gas sampling, and discloses a high-purity gas sampling method.The high-purity gas sampling system comprises a purging unit, the purging unit is communicated with a collecting unit through a connecting pipeline and used for inflating the collecting unit, the purging unit introduces purging gas through the outside, and the purging gas is inert gas; the sampling unit is communicated with the connecting pipeline and is used for filling sampling gas into the collecting unit; the air inlet end of the collecting unit is connected with the connecting pipeline, and the air outlet end of the collecting unit is connected with the discharging pipeline. Silane in the pipeline is discharged through purging before bottle replacement, so that the silane in the pipeline is prevented from encountering air, and the sampling safety is improved. And through purging after bottle replacement, air entering the pipeline is discharged, so that the air is prevented from entering the sampling bottle, and the sampling purity is increased.

Description

Technical Field

[0001] The invention relates to the field of gas sampling, and in particular to a high-purity gas sampling method and device. Background Art

[0002] Due to the production needs of the semiconductor industry, the requirements for gas purity are getting higher and higher, and it is necessary to improve the accuracy of detecting the metal impurity content in the gas.

[0003] At present, when sampling silane gas, most of the sampling gas is directly filled into the sampling bottle. However, this sampling amplification causes silane gas to be contained in the pipeline during sampling. Therefore, when the sampling bottle is replaced after sampling, the silane gas in the pipeline comes into contact with the air, which is easy to cause accidents. Moreover, after the bottle is replaced, the air will enter the pipeline when the bottle is replaced, resulting in the air in the pipeline entering the sampling bottle during sampling, affecting the purity of the sample. Summary of the invention

[0004] Therefore, the technical problem to be solved by the present invention is to prevent air from entering the sampling bottle, improve the sampling purity, prevent the silane in the pipeline from contacting with the air, and reduce the possibility of accidents.

[0005] The above technical problem is solved by the following technical solution: The present invention proposes a high-purity gas sampling method, wherein the sampling bottle has an absorption liquid, the sampling bottle is fed with gas through an air inlet butt joint, and the sampling bottle is exhausted through an air outlet butt joint, and the high-purity gas sampling method comprises the following steps: Purge before changing the bottle. The purge unit adds purge gas into the sampling bottle through the air inlet butt joint. The gas in the sampling bottle is discharged through the air outlet butt joint, and the silane gas in the sampling device and the sampling bottle is discharged; After the bottle is changed, the purge unit adds purge gas into the sampling bottle through the air inlet butt joint, and the gas in the sampling bottle is discharged through the air outlet butt joint, and the air in the sampling device and the sampling bottle is discharged; For sampling, the sampling unit adds a quantitative amount of silane gas into the sampling bottle through the air inlet butt joint.

[0006] In a preferred embodiment of the high-purity gas sampling method of the present invention: in the step based on the purging before bottle change, after detecting that the pressure of the purging unit reaches the purging pressure setting value, it is stabilized for a period of 5 to 10 seconds, and the purging unit is closed to discharge the purging gas in the sampling bottle, and the discharge is terminated when the pressure in the sampling bottle is ≤2psi.

[0007] In a preferred embodiment of the high-purity gas sampling method of the present invention: in the step of purging after bottle replacement, after detecting that the pressure of the purge unit reaches the purge pressure setting value, it is stabilized for 5 to 10 seconds, and the purge unit is closed to discharge the purge gas in the sampling bottle. The discharge ends after 15 seconds, and the above is one cycle.

[0008] In a preferred embodiment of the high-purity gas sampling method of the present invention: in the step of purging after changing the bottle, the number of cycles can be set, and the number of cycles is 3 times.

[0009] In a preferred embodiment of the high-purity gas sampling method of the present invention, the following steps are also included: Positive pressure maintenance after bottle change: After the purging step before bottle change is completed, connect a new sampling bottle, open the purging unit, detect that the pressure in the sampling bottle reaches 10psi and stabilizes for 5 to 10 seconds, close the purging unit, and maintain the pressure for 12 to 24 hours. After the positive pressure maintenance step after bottle change is completed, enter the purging step after bottle change.

[0010] The present invention provides a high-purity gas sampling device, comprising: A purge unit, which is connected to the collecting unit through a connecting pipeline and is used to inflate the collecting unit. The purge unit introduces purge gas from the outside, and the purge gas is an inert gas; A sampling unit, which is connected to the connecting pipeline and is used to fill the collecting unit with sampling gas; The air inlet end of the collecting unit is connected to the connecting pipeline, and the air outlet end of the collecting unit is connected to the exhaust pipeline.

[0011] In a preferred embodiment of the high-purity gas sampling device of the present invention: the collection unit includes two sampling bottles, the two sampling bottles are connected in series through a series pipeline, a bypass pipeline is connected between the series pipeline and the exhaust pipeline, and a bypass pneumatic valve is arranged on the bypass pipeline.

[0012] In a preferred embodiment of the high-purity gas sampling device of the present invention: a self-cleaning pipeline is connected between the purge unit and the sampling unit, and a self-cleaning pneumatic valve is arranged on the self-cleaning pipeline.

[0013] In a preferred embodiment of the high-purity gas sampling device of the present invention: the purge unit includes a purge pipeline, a manual valve arranged on the purge pipeline, a pneumatic valve arranged on the purge pipeline, a flow controller arranged on the purge pipeline, a one-way valve arranged on the purge pipeline, a pneumatic valve arranged on the purge pipeline, and a pressure sensor arranged on the purge pipeline.

[0014] In a preferred embodiment of the high-purity gas sampling device of the present invention: the sampling unit includes a sampling pipeline, two manual valves arranged on the sampling pipeline, three pneumatic valves arranged on the sampling pipeline, two flow controllers arranged on the sampling pipeline, two one-way valves arranged on the sampling pipeline, four pneumatic valves arranged on the sampling pipeline, and two pressure sensors arranged on the sampling pipeline.

[0015] In a preferred embodiment of the high-purity gas sampling device of the present invention: a pressure sensor three is arranged on the connecting pipeline, a one-way valve three is arranged on the connecting pipeline, and a pneumatic valve five is arranged on the connecting pipeline.

[0016] In a preferred embodiment of the high-purity gas sampling device of the present invention: a discharge pneumatic valve is arranged on the discharge pipeline, a one-way valve four is arranged on the discharge pipeline, and a discharge manual valve is arranged on the discharge pipeline.

[0017] In a preferred embodiment of the high-purity gas sampling device of the present invention: the sampling bottle is provided with an air inlet butt joint pipe and an air outlet butt joint pipe, and both the air inlet butt joint pipe and the air outlet butt joint pipe are provided with docking manual valves.

[0018] In a preferred embodiment of the high-purity gas sampling device of the present invention: one end of the air inlet butt joint is inserted into the bottom of the inner cavity of the sampling bottle, one end of the air outlet butt joint is inserted into the top of the inner cavity of the sampling bottle, one of the air inlet butt joint is connected to the connecting pipeline, and one of the air outlet butt joint is connected to the discharge pipeline.

[0019] In a preferred embodiment of the high-purity gas sampling device of the present invention: the gas inlet butt joint pipe and the gas outlet butt joint pipe are both PFA sampling tubes.

[0020] The beneficial effects of the present invention are as follows: by purging before changing the bottle, the silane in the pipeline is discharged, the silane in the pipeline is prevented from encountering air, and the safety of sampling is increased. By purging after changing the bottle, the air entering the pipeline is discharged, the air is prevented from entering the sampling bottle, and the purity of the sampling is increased. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments of the present invention are briefly introduced below. Obviously, the drawings described below only relate to some embodiments of the present invention, but are not intended to limit the present invention. Among them: Figure 1 shows the overall schematic diagram of the high-purity gas sampling device; Figure 2 A schematic structural diagram of a purge unit is shown; Figure 3 shows a schematic structural diagram of a sampling unit; Figure 4 A schematic diagram showing the structural connection of a collecting unit as a sampling bottle is shown; Figure 5 A schematic diagram showing the structural connection of the collecting unit as two sampling bottles is shown; Figure 6 A schematic diagram of the connection of the bypass pipeline is shown; Figure 7 A schematic diagram of gas flow during self-cleaning of the device is shown; Figure 8 A schematic diagram showing the gas flow when one sampling bottle is used among two sampling bottles. DETAILED DESCRIPTION

[0022] In order to enable those skilled in the art to better understand the present invention, the present invention is further described in detail below in conjunction with specific implementation methods and drawings.

[0023] The terms used in the present invention are those general terms currently widely used in the art in consideration of the functions of the present invention, but these terms may vary according to the intention of a person of ordinary skill in the art, precedents, or new technologies in the art. In addition, specific terms may be selected by the applicant, and in this case, their detailed meanings will be described in the detailed description of the present invention. Therefore, the terms used in the specification should not be understood as simple names, but rather as a general description based on the meaning of the terms and the present invention.

[0024] Reference Figure 1 This embodiment provides a high-purity gas sampling device, including a purge unit 100, a sampling unit 200 and a collection unit 300.

[0025] The purge unit 100 is connected to the collection unit 300 through a connecting pipe 401, and is used to inflate the collection unit 300. The purge unit 100 introduces purge gas from the outside, and the purge gas is an inert gas. The sampling unit 200 is connected to the connecting pipe 401, and is used to fill the collection unit 300 with sampling gas. The air inlet end of the collection unit 300 is connected to the connecting pipe 401, and the air outlet end of the collection unit 300 is connected to the exhaust pipe 501.

[0026] Next, the purge unit 100 will be described.

[0027] One end of the purge unit 100 is an air inlet end, which is connected to a vacuum pump, and the vacuum pump is used to deliver the inert gas into the collection unit 300. The other end of the purge unit 100 is an air outlet end, which is connected to a connecting pipe 401, so that the purge unit 100 can deliver the inert gas into the collection unit 300 through the connecting pipe 401.

[0028] Reference Figure 2The purge unit 100 includes a purge pipeline 101 and control elements arranged on the purge pipeline 101, and the control elements include a manual valve 102, a pneumatic valve 103, a flow controller 105, a one-way valve 106, a pneumatic valve 107 and a pressure sensor 104.

[0029] One end of the purge line 101 is connected to the vacuum pump for air intake, and the other end is connected to the connecting line 401 for air outlet. Manual valve 102 is a backup control point, which can manually adjust the flow of gas when necessary, allowing manual intervention when there is a problem with the automatic control system. Pneumatic valve 103 controls the opening and closing of the valve through a pneumatic actuator to achieve automatic control of gas flow, ensure accurate control of gas flow, and improve the automation level of the system. Flow controller 105 adjusts and controls the gas flow through the purge line 101 to ensure the stability of the gas flow during the purge process and improve the purge efficiency and quality. Check valve 106 allows gas to flow in only one direction to prevent gas backflow and protect other components in the system, such as pressure sensors and pneumatic valves, from damage due to gas backflow. Pneumatic valve 2 107 is a redundant design to reduce the risk of failure of the entire system due to failure of a single component. When pneumatic valve 103 fails, pneumatic valve 2 107 can immediately take over its function to ensure the normal operation of the system. The pressure sensor 104 monitors the pressure in the purge line 101 to ensure that the pressure is maintained within a set safe and effective range and provide real-time pressure feedback.

[0030] Reference Figure 2 The vacuum pump passes the inert gas through one end of the purge pipe 101 as Figure 2 The B end shown in FIG. is filled into the purge pipeline 101, and the purge pipeline 101 is opened by opening the manual valve 102, the pneumatic valve 103 and the pneumatic valve 2 107, so that the inert gas can pass through the other end of the purge pipeline 101 as shown in FIG. Figure 2 The A end shown in FIG. 4 enters the connecting pipe 401 , and the inert gas enters the collecting unit 300 through the connecting pipe 401 to achieve a purge function.

[0031] Next, the sampling unit 200 will be described.

[0032] Reference Figure 3 One end of the sampling unit 200 is an air inlet end, which is connected to a silane pipeline. The silane pipeline is used to transport silane gas. The silane gas is delivered into the sampling unit 200 through the silane pipeline. The other end of the sampling unit 200 is an air outlet end, which is connected to a connecting pipeline 401, so that the sampling unit 200 can deliver the silane gas into the collecting unit 300 through the connecting pipeline 401.

[0033] The sampling unit 200 includes a sampling pipeline 201 and control elements arranged on the sampling pipeline 201, and the control elements include a manual valve 202, a pneumatic valve 3 203, a flow controller 205, a check valve 206, a pneumatic valve 4 207 and a pressure sensor 204.

[0034] One end of the sampling line 201 is connected to the silane line for the entry of silane gas, and the other end is connected to the connecting line 401 for the outlet. Manual valve 2 202 is a backup control point, which can manually adjust the flow of gas when necessary, allowing manual intervention when there is a problem with the automatic control system. Pneumatic valve 3 203 controls the opening and closing of the valve through a pneumatic actuator to achieve automatic control of gas flow, ensure accurate control of gas flow, and improve the automation of the system. Flow controller 2 205 adjusts and controls the gas flow through the sampling line 201 to ensure the stability of the gas flow during the sampling process and improve the sampling efficiency and quality. Check valve 2 206 allows gas to flow in only one direction to prevent gas backflow and protect other components in the system, such as pressure sensors and pneumatic valves, from damage due to gas backflow. Pneumatic valve 4 207 is a redundant design to reduce the risk of failure of the entire system due to failure of a single component. When pneumatic valve 3 203 fails, pneumatic valve 4 207 can immediately take over its function to ensure the normal operation of the system. The second pressure sensor 204 monitors the pressure in the sampling line 201 to ensure that the pressure is maintained within a set safe and effective range and provide real-time pressure feedback.

[0035] Next, the functions of flow controller 1 105 and flow controller 2 205 are explained.

[0036] Flow controller 105 is mainly used to control the flow rate of purge gas. During the purge process, it is necessary to ensure that the purge gas can enter the sampling bottle at a stable flow rate to achieve the purpose of replacing the residual gas, and it mainly plays the role of flow monitoring. Moreover, the flow rate of the purge gas of flow controller 105 is usually large to ensure rapid replacement. Since the flow rate of the purge gas is usually large, the flow range of flow controller 105 is wide, for example, from 0 to 1000 mL / min. During the purge process, the accuracy requirement of the flow rate is relatively low, and the main purpose is to ensure that the gas can be replaced quickly, so the accuracy of flow controller 105 may be around ±5%.

[0037] Flow controller 205 is mainly used to control the flow rate of the sampling gas. During the sampling process, the flow rate of the sampling gas needs to be accurately controlled to ensure that the collected gas sample is representative. It mainly controls the amount of sampling gas. The flow rate of the sampling gas is usually small to ensure the accuracy and safety of the sampling process. Since the flow rate of the sampling gas is usually small, the flow range of the flow controller 205 may be narrow, for example, from 0 to 500 mL / min. During the sampling process, the accuracy of the flow rate is required to be high to ensure that the collected gas sample is representative, so the accuracy of the flow controller 205 may be around ±1%.

[0038] Reference Figure 3 Silane gas passes through one end of the sampling pipeline 201 (such as Figure 3 The sampling pipeline 201 is opened by opening the manual valve 202, the pneumatic valve 3 203 and the pneumatic valve 4 207, so that the silane gas can pass through the other end of the sampling pipeline 201 (such as Figure 3 The C end shown in FIG. 4A ) enters the connecting pipe 401, and the silane gas enters the collecting unit 300 through the connecting pipe 401, thereby realizing the sampling function.

[0039] Next, the first situation of the collection unit 300 is described.

[0040] Reference Figure 4 One end of the collecting unit 300 is an inlet end for the inlet of inert gas or silane gas, and the other end is an outlet end for the outlet of inert gas or air.

[0041] The collection unit 300 includes a sampling bottle 301 , an air inlet butt joint 302 , an air outlet butt joint 303 and a butt joint manual valve 304 .

[0042] Among them, the sampling bottle 301 stores an absorption liquid, and the absorption liquid is used to absorb silane gas for subsequent detection of the purity of the silane gas. The air inlet butt joint 302 is used to connect with the connecting pipeline 401, so that the inert gas or silane gas can enter the sampling bottle 301 through the connecting pipeline 401. The end of the air inlet butt joint 302 is inserted into the bottom of the inner cavity of the sampling bottle 301, so that the gas can fully contact with the absorption liquid. The end of the air outlet butt joint 303 is inserted into the top of the inner cavity of the sampling bottle 301, so that the excess gas can be discharged through the air outlet butt joint 303. The butt end of the air inlet butt joint 302 and the connecting pipeline 401 (such as Figure 4 The butt end of the outlet butt pipe 303 and the discharge pipe 501 (such as Figure 4 F end in the middle).

[0043] The upper parts of the air outlet butt joint 303 and the air inlet butt joint 302 are made of stainless steel, which is convenient for installing the manual valve 304. The lower parts are PFA sampling tubes, which are convenient for inserting into the sampling bottle 301. Moreover, the material of the PFA sampling tube can avoid the entry of metal during friction, thereby ensuring the purity of the sampling.

[0044] Next, the second situation of the collection unit 300 is described.

[0045] Reference Figure 5 One end of the collecting unit 300 is an inlet end for the inlet of inert gas or silane gas, and the other end is an outlet end for the outlet of inert gas or air.

[0046] The collection unit 300 includes two sampling bottles 301 , an air inlet butt joint pipe 302 , an air outlet butt joint pipe 303 and a butt joint manual valve 304 .

[0047] The two sampling bottles 301 are connected in series via a series pipe 305. The outlet butt joint 303 on one sampling bottle 301 is connected in series with the inlet butt joint 302 on the other sampling bottle 301 via a series pipe 305. The two sampling bottles 301 connected in series have only one inlet end and one outlet end. Therefore, the inert gas or silane gas can only pass through the two sampling bottles 301 in sequence. The gas flow direction is as follows: Figure 5 As indicated by the arrow.

[0048] The sampling bottle 301 stores an absorption liquid, which is used to absorb silane gas for subsequent detection of the purity of the silane gas. The air inlet butt joint 302 is used to connect with the connecting pipeline 401, so that the inert gas or silane gas can enter the sampling bottle 301 through the connecting pipeline 401. The end of the air inlet butt joint 302 is inserted into the bottom of the inner cavity of the sampling bottle 301, so that the gas can fully contact with the absorption liquid. The end of the air outlet butt joint 303 is inserted into the top of the inner cavity of the sampling bottle 301, so that the excess gas can be discharged through the air outlet butt joint 303. The butt end of the air inlet butt joint 302 and the connecting pipeline 401 (such as Figure 5 The butt end of the outlet butt pipe 303 and the discharge pipe 501 (such as Figure 5 F end in the middle).

[0049] The upper parts of the air outlet butt joint 303 and the air inlet butt joint 302 are made of stainless steel, which is convenient for installing the manual valve 304. The lower parts are PFA sampling tubes, which are convenient for inserting into the sampling bottle 301. Moreover, the material of the PFA sampling tube can avoid the entry of metal during friction, thereby ensuring the purity of the sampling.

[0050] Next, the connection line 401 will be described.

[0051] Reference Figure 6A pressure sensor three 402 is provided on the connecting pipeline 401 , a one-way valve three 403 is provided on the connecting pipeline 401 , and a pneumatic valve five 404 is provided on the connecting pipeline 401 .

[0052] Among them, one end of the purge unit 100 is connected to the connecting pipe 401, so that the gas of the purge unit 100 can enter the sampling bottle 301 through the connecting pipe 401. One end of the sampling unit 200 is connected to the connecting pipe 401, so that the sampling gas can enter the sampling bottle 301 through the connecting pipe 401 to ensure the normal operation of the device.

[0053] The setting of the pressure sensor three 402 can detect the pressure of the gas in the connecting pipeline 401. Since the sampling bottle 301 is connected to the connecting pipeline 401, the pressure sensor three 402 can detect the pressure in the sampling bottle 301 to ensure the safety of sampling. At the same time, it can detect the pressure in the sampling bottle 301 during purging, and can also detect the pressure in the sampling bottle 301 during sampling. Detecting the pressure in the sampling bottle 301 during purging can prevent the purging pressure from being too low, thereby ensuring that the purging is clean. Detecting the pressure in the sampling bottle 301 during sampling can help confirm whether the sampling bottle 301 is well sealed. If the pressure in the bottle is abnormally reduced, it may indicate a leak.

[0054] The setting of the one-way valve 403 allows the purge gas or the sampling gas to enter the collection unit 300 only through the connecting pipe 401, preventing the gas in the collection unit 300 from flowing back, thereby ensuring the safety of the purge unit 100 and the sampling unit 200.

[0055] The setting of the pneumatic valve 5 404 can control the flow of the connecting pipeline 401, and cooperate with the pneumatic valves in the purge unit 100 and the sampling unit 200 to ensure the safety of the device.

[0056] Next, the exhaust line 501 will be described.

[0057] Reference Figure 6 A discharge pneumatic valve 502 is provided on the discharge pipeline 501, a one-way valve 503 is provided on the discharge pipeline 501, and a discharge manual valve 504 is provided on the discharge pipeline 501.

[0058] The exhaust pipeline 501 is communicated with the exhaust end of the collection unit 300 , so that the gas in the collection unit 300 can be exhausted through the exhaust pipeline 501 .

[0059] The setting of the discharge pneumatic valve 502 can control the flow of the discharge pipeline 501 and increase the automation of the device. The setting of the one-way valve 503 allows the gas in the collection unit 300 to flow out only through the discharge pipeline 501, and the gas in the discharge pipeline 501 will not flow back to the collection unit 300, thereby ensuring the sampling purity of the collection unit 300.

[0060] The setting of the discharge manual valve 504 cooperates with the discharge pneumatic valve 502 to prevent the discharge pneumatic valve 502 from being damaged and unable to control the flow of the discharge pipeline 501, thereby ensuring the safety of the device.

[0061] Next, the self-cleaning pipeline 601 will be described.

[0062] Reference Figure 6 A self-cleaning pipeline 601 is connected between the purge unit 100 and the sampling unit 200 , and a self-cleaning pneumatic valve 602 is arranged on the self-cleaning pipeline 601 .

[0063] One end of the self-cleaning pipeline 601 is connected to the purge pipeline 101, and the connection end is located downstream of the one-way valve 106. The other end of the self-cleaning pipeline 601 is connected to the sampling pipeline 201, and is located upstream of the one-way valve 206.

[0064] The setting of the self-cleaning pneumatic valve 602 can control the flow of the self-cleaning pipeline 601, so that the device opens the self-cleaning pneumatic valve 602 when the pipeline needs to be cleaned.

[0065] When the device needs to clean the pipeline in the sampling unit 200, open the self-cleaning pneumatic valve 602, and purge gas such as Figure 7 The liquid flows in the direction indicated by the arrow to clean the pipes in the device.

[0066] Next, the series line 305 and the bypass line 306 will be described.

[0067] Reference Figure 6 The two sampling bottles 301 are connected in series through a series pipeline 305 , a bypass pipeline 306 is connected between the series pipeline 305 and the discharge pipeline 501 , and a bypass pneumatic valve 307 is provided on the bypass pipeline 306 .

[0068] By setting the series pipeline 305, the two sampling bottles 301 are connected, so when performing a purging operation, the two sampling bottles 301 can be purged at the same time, and when performing a sampling operation, the two sampling bottles 301 can be sampled at the same time, thereby increasing the sampling efficiency of the device.

[0069] By setting the bypass line 306 and the bypass pneumatic valve 307, the bypass pneumatic valve 307 can control the flow of the bypass line 306. Therefore, when two bottles of samples need to be sampled, the bypass pneumatic valve 307 is closed to connect the two sampling bottles 301 in series, so that the two sampling bottles 301 can be sampled at the same time. When only one bottle of sample is needed, the bypass pneumatic valve 307 is opened, and the gas flows to Figure 8 As shown by the arrow, the device can operate on a sampling bottle 301. Through the setting of the bypass pipeline 306 and the bypass pneumatic valve 307, the device can choose to sample one or two bottles of samples according to demand.

[0070] This embodiment provides a high-purity gas sampling method, and the sampling process is as follows.

[0071] Purge before changing bottles: Open the purge unit 100 and add purge gas into the sampling bottle 301 through the air inlet butt joint 302. The gas in the sampling bottle 301 is discharged through the discharge pipeline 501. After the pressure of the purge unit 100 reaches the purge pressure setting value and stabilizes for 5 to 10 seconds, close the purge unit 100. Discharge the purge gas in the sampling bottle 301 until the pressure in the sampling bottle 301 is ≤2psi.

[0072] Among them, during the gas replacement and purging process, a certain residence time is usually required to ensure the uniform distribution and replacement effect of the gas. Therefore, it is necessary to ensure that after the gas pressure in the system reaches the set value, there is enough residence time for the gas to be fully replaced and stabilized. During the purging process, a stabilization time of 5 to 10 seconds can ensure that the purge gas fully enters the sampling bottle 301 and the pipeline to replace the original gas (such as silane gas or air). If the time is too short, it may not be completely replaced, resulting in residual gas affecting the purity of subsequent sampling.

[0073] Table 1 shows the residual gas concentration in the sampling bottle 301 at different purge times.

[0074] Table 1 Comparison of purge time and residual concentration Experiment number Stabilization time (seconds) Residual silane gas concentration after purging before changing the bottle (ppm) Residual air concentration after purging after bottle change (ppm) Gas purity after sampling (%) 1 5 2.3 1.5 99.5 2 7 1.8 1.2 99.6 3 10 1.5 1 99.7 4 15 1.4 0.9 99.7 5 20 1.3 0.8 99.8

[0075] From 5 seconds to 20 seconds, the residual silane gas concentration gradually decreased, and the residual air concentration also gradually decreased, indicating that the longer the stabilization time, the better the replacement effect. At 10 seconds, the residual silane gas concentration was 1.5 ppm and the residual air concentration was 1.0 ppm, which were already low. Continuing to increase the stabilization time to 15 seconds and 20 seconds, the residual concentration was further reduced, but the effect was not obvious.

[0076] Among them, when the pressure in the sampling bottle 301 drops below 2psi, the gas pressure in the bottle is close to the external atmospheric pressure (about 14.7 psi), which can effectively prevent gas leakage. Especially for flammable and explosive gases such as silane, ensuring low pressure can significantly reduce safety risks. If the pressure in the sampling bottle 301 is too low (for example, below atmospheric pressure), it may cause external air to flow back into the sampling bottle 301, thereby polluting the sampling environment and affecting the sampling purity. This situation can be avoided by controlling the pressure at about 2psi. During the purge process, the gas in the sampling bottle 301 is discharged to a pressure of ≤2psi, which can ensure that the gas in the sampling bottle 301 is fully replaced. If the pressure is too high, some residual gas may not be completely discharged, thereby affecting the purity of subsequent sampling. By controlling the pressure at about 2psi, the amount of purge gas used can be effectively reduced while ensuring the replacement effect. If the pressure is too low (such as close to vacuum), more purge gas is required to achieve the same replacement effect, which not only increases the cost, but also may cause unnecessary burden on the equipment.

[0077] Therefore, the purge time can be stabilized at 5 to 10 seconds. A purge time that is too short will result in an inability to purge thoroughly. A purge time that is too long will not only affect the sampling efficiency, but also waste purge gas. Moreover, the marginal benefit of purge longer than 10 seconds is low.

[0078] After sampling is completed, purge gas is added into the sampling bottle 301 through the purge unit 100 to discharge the unabsorbed silane gas in the sampling bottle 301 and the silane gas in the pipeline, thereby preventing silane from contacting with air and improving the safety of sampling.

[0079] By first filling to a set pressure, then closing the purge unit 100 and opening the exhaust port, it is ensured that there is enough gas to remove impurities in the sampling bottle 301 during the purge process. This can improve the purge efficiency and ensure that the gas in the sampling bottle 301 is fully replaced.

[0080] After the sampling bottle 301 is filled with gas to reach a certain pressure value, the gas in the sampling bottle 301 is then discharged. Through the operation of inflation and deflation, the amount of inert gas used is reduced compared to continuous inflation and circulation. Moreover, through the operation of inflation and deflation, the gas discharged by the device is a mixture of silane gas and inert gas, rather than pure silane gas, which increases the safety of the device during exhaust. Moreover, through the operation of inflation and deflation, the silane gas in the pipeline can be added to the sampling bottle 301, which reduces the waste of silane gas compared to continuous gas circulation.

[0081] By purging before changing the bottle, not only is it ensured that there is no silane gas in the pipeline, ensuring the safety of the operation, but the discharge is terminated when the pressure in the sampling bottle 301 is ≤2psi, ensuring the pressure in the sampling bottle 301 and facilitating the subsequent replacement of the sampling bottle 301.

[0082] The specific operation is: open the pneumatic valve 103 and the pneumatic valve 2 107 on the purge unit 100, open the pneumatic valve 5 404 on the connecting pipeline 401, at this time, the docking manual valve 304 is in the open state, the pressure sensor 104 and the pressure sensor 3 402 reach the purge pressure setting value, stabilize for a period of 5-10S, close the pneumatic valve 103 and the pneumatic valve 2 107, open the discharge pneumatic valve 502 to discharge, the pressure sensor 3 402 monitors the pressure in the sampling bottle 301 ≤ 2psi to end the discharge, and then close the discharge pneumatic valve 502; the above is one cycle. The number of replacements can be set.

[0083] When only one sampling bottle 301 needs to be sampled, the specific operation is: open the pneumatic valve 103 and the pneumatic valve 2 107 on the purge unit 100, open the pneumatic valve 5 404 on the connecting line 401, at this time, the docking manual valve 304 of the No. 1 sampling bottle 301 is in an open state, wherein the sampling bottle 301 connected to the connecting line 401 is the No. 1 sampling bottle 301, the manual valve of the No. 2 sampling bottle 301 is in a closed state, wherein the sampling bottle 301 connected to the discharge line 501 is the No. 2 sampling bottle 301, and at the same time open the bypass pneumatic valve 307, after the pressure sensor 1 104 and the pressure sensor 3 402 reach the purge pressure setting value, stabilize for a period of 5-10S, close the pneumatic valve 1 103 and the pneumatic valve 2 107, open the discharge pneumatic valve 502 to discharge, the pressure sensor 3 402 monitors the pressure in the sampling bottle 301 ≤2psi to end the discharge, and then close the discharge pneumatic valve 502; the above is one cycle. This number of replacements can be set.

[0084] Stabilizing for 5-10 seconds can not only observe whether the sampling bottle 301 is leaking, but also allow the gas in the system enough time to reach the set pressure value, which can more effectively remove impurities or residual gas in the system and improve the purge efficiency.

[0085] Replace the sampling bottle 301: After the purging is completed before changing the bottle, close all pneumatic valves and manually close the docking manual valve 304. Remove the existing sampling bottle 301, install the new sampling bottle 301, and ensure that all joints are well sealed.

[0086] After the pre-bottle purging is completed, the sampling bottle 301 is replaced to prepare for new sampling.

[0087] After changing the bottle, maintain positive pressure: open the purge unit 100, and check that the pressure in the sampling bottle 301 reaches 10 psi and then stabilizes for 5 to 10 seconds. Close the purge unit 100, and maintain the pressure for 12 to 24 hours to ensure that the pressure in the sampling bottle 301 is stable.

[0088] The pressure value in the detection sampling bottle 301 can be set to be lower than the atmospheric pressure. In the negative pressure state, the pressure in the sampling bottle is lower than the external atmospheric pressure, which can effectively prevent the gas in the sampling bottle from leaking. In particular, for flammable and explosive gases (such as silane), negative pressure can significantly reduce the risk of gas leakage.

[0089] After the pressure in the sampling bottle 301 is detected, it needs to be stabilized for 5 to 10 seconds. The stabilization time can be set. A short stabilization time can ensure uniform pressure in the system and prevent the pressure value in the sampling bottle 301 from being different from that at the detection point.

[0090] Maintaining the pressure for 12 to 24 hours can ensure that the pressure in the sampling bottle 301 remains stable for a long time. This step can detect the sealing of the sampling bottle 301 and the entire system to ensure that the sampling purity will not be affected by leakage during the subsequent sampling process.

[0091] After replacing the new sampling bottle 301 , the sampling bottle 301 is inflated through the purging unit 100 to ensure that the pressure in the sampling bottle 301 reaches and remains at a certain level, thereby preventing external air from entering, and at the same time, the new sampling bottle 301 is tested for sealing.

[0092] The specific operation is: open the pneumatic valve 103 and the pneumatic valve 2 107 on the purge unit 100, open the pneumatic valve 5 404 on the connecting pipe 401, at this time the docking manual valve 304 is in the open state, close the exhaust pneumatic valve 502, the pressure sensor 3 402 monitors the pressure in the sampling bottle 301 and stops adding gas to the sampling bottle 301 when it reaches 10psi, and at the same time close the pneumatic valve 103 and the pneumatic valve 2 107 to maintain the pressure for 12-24 hours.

[0093] Similarly, when one sampling bottle 301 needs to be operated, the bypass pneumatic valve 307 is opened, and the docking manual valve 304 on the second sampling bottle 301 is closed.

[0094] Purge after bottle replacement: Open the purge unit 100 and add purge gas to the sampling bottle 301 through the air inlet butt joint 302. The gas in the sampling bottle 301 is discharged through the exhaust pipe 501. After the pressure of the purge unit 100 reaches the purge pressure setting value and stabilizes for 5 to 10 seconds, close the purge unit 100. The purge gas in the sampling bottle 301 is discharged for 15 seconds and then the discharge is terminated.

[0095] The main purpose of purging after changing the bottle is to discharge the air that may remain in the sampling bottle 301 and the pipeline, to ensure the purity of the gas in the sampling bottle 301, and to prevent the air from affecting the sampling results. Since purging after changing the bottle only requires replacing the control, it is not necessary to ensure that the pressure in the sampling bottle 301 is higher or lower than the atmospheric pressure, so it is only necessary to discharge the purge gas, and the setting of the discharge time of 15 seconds can ensure that the air in the sampling bottle 301 is discharged cleanly.

[0096] The purge gas discharge time in the sampling bottle 301 can be set and determined according to the first discharge time. For example, after the pressure of the purge unit 100 reaches the purge pressure setting value, it is stable for 5 to 10 seconds and the purge unit 100 is turned off. The purge gas in the sampling bottle 301 is discharged for a period of time and recorded. The recorded time is the discharge time. By accurately setting the discharge time, it can be prevented that the time is too short to cause incomplete discharge, and it can also be prevented that the time is too long to affect the sampling efficiency.

[0097] In the step of purging after bottle change, the number of cycles can be set.

[0098] During the gas replacement process, as the number of cycles increases, the effect of each cycle on the purity improvement and residual air concentration reduction gradually decreases. In the first few cycles, each cycle can significantly improve the replacement effect. However, when the number of cycles increases to a certain extent, the improvement effect brought by each cycle becomes very limited, or even negligible.

[0099] The number of cycles and the residual air concentration in the sampling bottle 301 are described in Table 2 as follows.

[0100] Table 2 Comparison of cycle times and residual air concentration Experiment number Cycle times Residual air concentration (ppm) Purification gas purity (%) 1 1 50 98 2 2 20 99 3 3 10 99.5 4 4 8 99.6 5 5 6 99.7

[0101] From cycle 1 to cycle 3, the residual air concentration decreased by 40 ppm from 50 ppm to 10 ppm. The purge gas purity increased by 1.5% from 98.0% to 99.5%.

[0102] From 3 to 5 cycles, the residual air concentration decreased from 10 ppm to 6 ppm, a decrease of only 4 ppm. The purge gas purity increased from 99.5% to 99.7%, an increase of only 0.2%.

[0103] From 3 cycles to 5 cycles, the improvement brought by each cycle is very limited, and the improvement range of each cycle is basically the same, indicating that it has reached the stage of physical limits and diminishing marginal benefits.

[0104] Therefore, the number of cycles can be set to 3 times. 3 cycles can significantly reduce the residual air concentration and improve the gas purity. The improvement effect brought by further increasing the number of cycles is very limited and it is not worth adding more resources and time costs.

[0105] After the positive pressure is maintained after the bottle is replaced, the purge gas is added to the sampling bottle 301 again through the purge unit 100 to expel the air that may remain in the sampling bottle 301 and the pipeline, ensuring that the gas in the sampling bottle 301 is pure and avoiding the air from affecting the sampling result.

[0106] The specific operation is: open the pneumatic valve 103 and the pneumatic valve 2 107 on the purge unit 100, open the pneumatic valve 5 404 on the connecting pipeline 401, at this time, the docking manual valve 304 is in the open state, after the pressure sensor 104 and the pressure sensor 3 402 reach the purge pressure setting value, stabilize for a period of 5-10S, close the pneumatic valve 103 and the pneumatic valve 2 107, open the discharge pneumatic valve 502 to discharge, discharge the purge gas in the sampling bottle 301 for 15 seconds and then end the discharge; the above is one cycle. This replacement number can be set.

[0107] Similarly, when one sampling bottle 301 needs to be operated, the bypass pneumatic valve 307 is opened, and the docking manual valve 304 on the second sampling bottle 301 is closed.

[0108] By purging multiple times before and after changing bottles, use high-purity inert gases such as helium or nitrogen to purge the residual gas and possible impurities in the system to ensure the cleanliness of the sampling environment.

[0109] Sampling: Open the sampling unit 200 and add a certain amount of silane gas into the sampling bottle 301 through the gas inlet butt joint 302. When the sampling flow rate reaches the set sampling amount, close the sampling unit 200.

[0110] A certain amount of silane gas is added from the sampling unit 200 into the sampling bottle 301 to collect the required gas sample for subsequent analysis and detection.

[0111] The specific operation is: manually open the manual valve 202 on the sampling unit 200, and the silane gas enters through the sampling pipeline 201, open the pneumatic valve 207 and the pneumatic valve 3 203 on the sampling unit 200, and open the pneumatic valve 5 404 on the connecting pipeline 401. At this time, the docking manual valve 304 is in an open state, and the silane gas dissolves into the solution in the sampling bottle 301, so as to collect the silane gas, set the pressure value through the pressure sensor 204, and control the amount of silane gas added to the sampling bottle 301 through the flow controller. When the sampling flow reaches the set sampling amount, close all pneumatic valves, and automatically jump to the purge before changing the bottle to enter the next cycle.

[0112] Finally, it should be pointed out that the methods and devices described in detail above are only embodiments, and those skilled in the art can modify these embodiments in different ways without departing from the scope of the present invention.

Claims

1. A high-purity gas sampling device, characterized in that: include, A purge unit (100) is connected to the collection unit (300) via a connecting pipeline (401) and is used to inflate the collection unit (300), wherein the purge unit (100) introduces purge gas from the outside, and the purge gas is an inert gas; A sampling unit (200), which is connected to the connecting pipeline (401) and is used to fill the collection unit (300) with sampling gas; The air inlet end of the collection unit (300) is connected to the connecting pipeline (401), and the air outlet end of the collection unit (300) is connected to the exhaust pipeline (501).

2. The high-purity gas sampling device according to claim 1, characterized in that: The collection unit (300) comprises two sampling bottles (301), the two sampling bottles (301) are connected in series via a series pipeline (305), a bypass pipeline (306) is connected between the series pipeline (305) and the discharge pipeline (501), and a bypass pneumatic valve (307) is provided on the bypass pipeline (306).

3. The high-purity gas sampling device according to claim 1, characterized in that: A self-cleaning pipeline (601) is connected between the purge unit (100) and the sampling unit (200), and a self-cleaning pneumatic valve (602) is arranged on the self-cleaning pipeline (601).

4. The high-purity gas sampling device according to any one of claims 1 to 3, characterized in that: The purge unit (100) comprises a purge pipeline (101), a manual valve (102) arranged on the purge pipeline (101), a pneumatic valve (103) arranged on the purge pipeline (101), a flow controller (105) arranged on the purge pipeline (101), a one-way valve (106) arranged on the purge pipeline (101), a pneumatic valve (107) arranged on the purge pipeline (101), and a pressure sensor (104) arranged on the purge pipeline (101).

5. The high-purity gas sampling device according to any one of claims 1 to 3, characterized in that: The sampling unit (200) comprises a sampling pipeline (201), a second manual valve (202) arranged on the sampling pipeline (201), a third pneumatic valve (203) arranged on the sampling pipeline (201), a second flow controller (205) arranged on the sampling pipeline (201), a second one-way valve (206) arranged on the sampling pipeline (201), a fourth pneumatic valve (207) arranged on the sampling pipeline (201), and a second pressure sensor (204) arranged on the sampling pipeline (201).

6. The high-purity gas sampling device according to any one of claims 1 to 3, characterized in that: The connecting pipeline (401) is provided with a pressure sensor three (402), the connecting pipeline (401) is provided with a one-way valve three (403), and the connecting pipeline (401) is provided with a pneumatic valve five (404).

7. The high-purity gas sampling device according to claim 6, characterized in that: The discharge pipeline (501) is provided with a discharge pneumatic valve (502), the discharge pipeline (501) is provided with a one-way valve four (503), and the discharge pipeline (501) is provided with a discharge manual valve (504).

8. The high-purity gas sampling device according to claim 2, characterized in that: The sampling bottle (301) is provided with an air inlet butt joint pipe (302) and an air outlet butt joint pipe (303), and both the air inlet butt joint pipe (302) and the air outlet butt joint pipe (303) are provided with a butt joint manual valve (304).

9. The high-purity gas sampling device according to claim 8, characterized in that: One end of the air inlet butt joint (302) is inserted into the bottom of the inner cavity of the sampling bottle (301), and one end of the air outlet butt joint (303) is inserted into the top of the inner cavity of the sampling bottle (301). One of the air inlet butt joint (302) is connected to the connecting pipeline (401), and one of the air outlet butt joint (303) is connected to the exhaust pipeline (501).

10. The high-purity gas sampling device according to claim 9, characterized in that: The air inlet butt joint pipe (302) and the air outlet butt joint pipe (303) both adopt PFA sampling tubes.

11. A high-purity gas sampling method, characterized in that: Applicable to the high-purity gas sampling device as claimed in any one of claims 1 to 10, the sampling bottle (301) contains an absorbing liquid, the sampling bottle (301) takes in air through an air inlet butt joint (302), and the sampling bottle (301) exhausts air through an air outlet butt joint (303), and the high-purity gas sampling method comprises the following steps: Purging before changing the bottle, the purging unit (100) adds purging gas into the sampling bottle (301) through the gas inlet butt joint (302), the gas in the sampling bottle (301) is discharged through the gas outlet butt joint (303), and the silane gas in the sampling device and the sampling bottle (301) is discharged; After the bottle is replaced, the purging unit (100) adds purging gas into the sampling bottle (301) through the air inlet butt joint (302), and the gas in the sampling bottle (301) is discharged through the air outlet butt joint (303), thereby discharging the air in the sampling device and the sampling bottle (301); Sampling: the sampling unit (200) adds a quantitative amount of silane gas into the sampling bottle (301) through the gas inlet butt joint (302).

12. The high-purity gas sampling method according to claim 11, characterized in that: In the step of purging before changing the bottle, after detecting that the pressure of the purge unit (100) reaches the purge pressure setting value, it is stabilized for a period of 5 to 10 seconds, and then the purge unit (100) is closed to discharge the purge gas in the sampling bottle (301), and the discharge is terminated when the pressure in the sampling bottle (301) is ≤2psi.

13. The high-purity gas sampling method according to claim 11, characterized in that: In the step of purging after bottle replacement, after detecting that the pressure of the purge unit (100) reaches the purge pressure setting value and stabilizes for 5 to 10 seconds, the purge unit (100) is closed and the purge gas in the sampling bottle (301) is discharged. The discharge ends after 15 seconds, and the above constitutes one cycle.

14. The high-purity gas sampling method according to claim 13, characterized in that: In the step of purging after changing the bottle, the number of cycles can be set, and the number of cycles is 3 times.

15. The high-purity gas sampling method according to any one of claims 11 to 13, characterized in that: The following steps are also included: Positive pressure maintenance after bottle change: After the purging step before bottle change is completed, a new sampling bottle (301) is connected, the purging unit (100) is opened, and the pressure in the sampling bottle (301) is detected to reach 10 psi and then stabilized for 5 to 10 seconds, the purging unit (100) is closed, and the pressure is maintained for 12 to 24 hours. After the positive pressure maintenance step after bottle change is completed, the purging step after bottle change is entered.

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