CN111665292B - High-pressure gas sampling test device and sampling test method - Google Patents
High-pressure gas sampling test device and sampling test method Download PDFInfo
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17D—PIPE-LINE SYSTEMS; PIPE-LINES
- F17D3/00—Arrangements for supervising or controlling working operations
- F17D3/10—Arrangements for supervising or controlling working operations for taking out the product in the line
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
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Abstract
The embodiment of the application provides a high-pressure gas sampling test device and a sampling test method, wherein the high-pressure gas sampling test device comprises a vacuum transition assembly, a vacuum measurement assembly and a sampling channel assembly; the vacuum transition assembly is used for decompressing and acquiring high-pressure gas to be detected with certain air pressure; the vacuum measurement assembly is used for measuring the gas composition of the high-pressure gas to be measured; the sampling channel component is used for connecting the vacuum transition component and/or the vacuum measurement component; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch. The high-pressure gas sampling test device and the sampling test method can systematically study and analyze the influence of one or more gas sampling modes on gas component analysis.
Description
Technical Field
The application belongs to the technical field of measurement and analysis, and particularly relates to a high-pressure gas sampling test device and a sampling test method.
Background
Extreme ultraviolet lithography (EUVL) is used to obtain lithography node technologies of 7nm and below, and extreme ultraviolet lithography machines employ Extreme Ultraviolet (EUV) light having a wavelength of 13.5nm, and the optics, wafer stage and mask stage of the extreme ultraviolet lithography machine must be in a vacuum environment because air and almost all refractive optical materials have a strong absorption effect on EUV13.5 nm. Any solid material is deflated when placed under vacuum environment, and the resist is reacted with during EUV exposure to generate large amounts of gasAn amount of a contaminating gas. The reflectors in the EUVL optical system are very sensitive to pollutants, and the reflectivity of the reflectors is reduced when the reflectors are slightly polluted, so that the EUVL system has strict requirements on the total pressure, the gas composition and the partial pressure of each vacuum microenvironment. Literature (AbneeshSrivastava, stenioPereira, thomas gaffney. Sub-Atmospheric Gas Purification for EUVL Vacuum Environment control. Spie, 2012) states that extreme ultraviolet lithography (EUVL) partial vacuum environments require hydrocarbon (CxHy) partial pressures of less than or equal to 1 x 10 -7 Pa, water partial pressure is less than or equal to 1 multiplied by 10 -5 Pa to ensure that the reflectance loss of the optical system is less than 1% over 7-10 years.
Mass spectrometers are commonly used in industry to achieve accurate measurements of gas composition and partial pressure in vacuum. Typical mass spectrometers require that a certain vacuum (e.g. 10 -2 Pa) which would otherwise cause damage to the mass spectrometer components. The total pressure of the EUVL vacuum micro-environment is about Pa magnitude low vacuum, which is higher than the working pressure of a general mass spectrometer, and the gas to be detected in vacuum needs to be subjected to depressurization sampling for detection; meanwhile, the partial pressure measurement of the EUVL vacuum microenvironment needs to react fast enough, and has certain requirements on sampling time.
The method for sampling the gas under the vacuum is many, such as capillary sampling, small hole sampling, sampling valves and the like, and the gas component analysis result is closely related to the sampling process, such as the pressure reduction measurement is used for obtaining the gas component proportion change condition, sampling time and the like, and the influence research of the sampling method on the gas component analysis is carried out, so that the more accurate vacuum gas analysis result is obtained. Therefore, there is a need for a high-pressure gas sampling test apparatus and a sampling test method that can systematically study the influence of a gas sampling system on gas component analysis.
Disclosure of Invention
The invention provides a sampling test device and a sampling test method for high-pressure gas, and aims to solve the problem that the influence of a gas sampling mode on gas component analysis needs to be systematically researched and analyzed in the existing high-pressure gas sampling analysis technology.
According to a first aspect of embodiments of the present application, there is provided a high-pressure gas sampling test apparatus, including a vacuum transition assembly, a vacuum measurement assembly, and a sampling channel assembly, in particular:
the vacuum transition assembly is used for decompressing and acquiring high-pressure gas to be detected with certain air pressure;
the vacuum measurement assembly is used for measuring the gas composition of the high-pressure gas to be measured;
the sampling channel component is used for connecting the vacuum transition component and/or the vacuum measurement component; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch.
Optionally, the vacuum transition assembly comprises a transition chamber, a vacuum gauge and a vacuum transition pump set; the front end of the transition chamber is directly decompressed to obtain or is connected with the sampling channel assembly and then decompressed to obtain the high-pressure gas to be tested, and the rear end of the transition chamber is connected with the sampling channel assembly or the vacuum measuring assembly; the transition chamber is connected with a vacuum gauge and a vacuum transition pump set.
Optionally, the vacuum measurement assembly comprises a mass spectrometry chamber, a vacuum gauge, a mass spectrometer and a vacuum measurement pump set; the front end of the mass spectrum chamber is directly acquired or connected with the sampling channel assembly to acquire vacuum to be measured with certain air pressure, and the mass spectrum chamber is connected with the vacuum gauge, the mass spectrometer and the vacuum measurement pump set.
Optionally, the vacuum transition pump set and the vacuum measurement pump set each comprise a molecular pump and a mechanical pump.
Optionally, the sampling channel branch comprises a sampling channel and a shut-off valve.
Optionally, the stop valve of the sampling channel branch is arranged at one end or two ends of the sampling channel.
Optionally, the sampling channel is removably mounted to the sampling channel branch.
Optionally, the device further comprises a fine tuning valve, wherein the fine tuning valve is arranged on a channel between the vacuum measuring assembly and the vacuum transition assembly or on a channel for obtaining high-pressure gas to be measured by decompression of the vacuum transition assembly.
According to a second aspect of the embodiments of the present application, there is provided a high-pressure gas sampling test method, specifically including the steps of:
decompressing to obtain high-pressure gas to be detected with certain air pressure;
measuring the gas composition of the high-pressure gas to be measured;
the method comprises the steps of obtaining high-pressure gas to be detected through a sampling channel assembly in a decompression mode, and/or obtaining the high-pressure gas to be detected with certain air pressure through the sampling channel assembly; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch.
Optionally, the sampling channel branch comprises a sampling channel and a shut-off valve.
By adopting the high-pressure gas sampling test device and the sampling test method in the embodiment of the application, the high-pressure gas sampling test device comprises a vacuum transition assembly, a vacuum measurement assembly and a sampling channel assembly; the vacuum transition assembly is used for decompressing and acquiring high-pressure gas to be detected with certain air pressure; the vacuum measurement assembly is used for measuring the gas composition of the high-pressure gas to be measured; the sampling channel component is used for connecting the vacuum transition component and/or the vacuum measurement component; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch. The high-pressure gas sampling test device and the sampling test method can systematically study and analyze the influence of one or more gas sampling modes on gas component analysis.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application. In the drawings:
a schematic structural diagram of a high pressure gas sampling test apparatus according to an embodiment of the present application is shown in fig. 1;
a schematic structural diagram of a high-pressure gas sampling test apparatus according to another embodiment of the present application is shown in fig. 2;
a schematic structural diagram of a high pressure gas sampling test apparatus according to another embodiment of the present application is shown in fig. 3;
FIG. 4 shows a schematic structural diagram of a high pressure gas sampling test apparatus according to another embodiment of the present application;
FIG. 5 illustrates a comparison of atmospheric mass spectra obtained from needle valve and capillary sampling in accordance with an embodiment of the present application;
FIG. 6 shows a comparison of isotope spectra of needle valve and capillary sampling to obtain trace Xe gas in the atmosphere in accordance with embodiments of the present application;
FIG. 7 shows a schematic step diagram of a high pressure gas sampling test method according to an embodiment of the present application;
the device comprises a 01-sampling valve, a 02-sampling capillary, a 03-sampling small hole, a 11-mass spectrum chamber, a 12-transition chamber, 21-22 mechanical pumps, 23-24 molecular pumps, 31-32 vacuum gauges, 33-mass spectrometers, 41-46, 410-stop valves, 47-three-way valves, 48-angle valves, 49-fine tuning valves, 411-416-stop valves, 51-sampling valves, 52-sampling capillary and 53-sampling small holes.
Detailed Description
In the process of realizing the application, the inventor finds that when the high-pressure gas is measured, the gas sampling modes, such as capillary sampling, small hole sampling, sampling valves and the like, are numerous, the gas component analysis result is closely related to the sampling process, and if the more accurate high-pressure gas analysis result is required to be obtained, the influence of the gas sampling mode on the gas component is required to be analyzed and researched, and then the gas analysis result is corrected to obtain the more accurate analysis result.
By adopting the high-pressure gas sampling test device and the sampling test method in the embodiment of the application, the sampling channel can be selected by adopting the sampling channel component. The sampling channel component is used for connecting the vacuum transition component and/or the vacuum measurement component; the vacuum transition assembly is used for decompressing and acquiring high-pressure gas to be detected with certain air pressure; the vacuum measurement component is used for indirectly measuring the gas composition of the high-pressure gas to be measured; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch. The high-pressure gas sampling test device and the sampling test method can systematically study and analyze the influence of one or more gas sampling modes on gas component analysis.
In order to make the technical solutions and advantages of the embodiments of the present application more apparent, the following detailed description of exemplary embodiments of the present application is given with reference to the accompanying drawings, and it is apparent that the described embodiments are only some of the embodiments of the present application and not exhaustive of all the embodiments. It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other.
Example 1
The embodiment of the application provides a high-pressure gas sampling test device includes vacuum transition subassembly, vacuum measurement subassembly and sampling channel subassembly, and is specific:
vacuum transition assembly: the device is used for decompressing and acquiring the high-pressure gas to be detected with certain air pressure.
Vacuum measurement assembly: and the gas composition is used for indirectly measuring the high-pressure gas to be measured.
Sampling channel assembly: for connecting the vacuum transition assembly and/or vacuum measurement assembly; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch.
In addition to the above components, optionally, the high-pressure gas sampling test device further comprises a fine tuning valve, wherein the fine tuning valve is arranged on a channel between the vacuum measurement component and the vacuum transition component or on a channel for obtaining high-pressure gas to be tested by decompression of the vacuum transition component.
The vacuum transition assembly comprises a transition chamber, a vacuum gauge and a vacuum transition pump set. The front end of the transition chamber is directly decompressed to obtain or is connected with the sampling channel assembly to obtain the high-pressure gas to be measured, and the rear end of the transition chamber is connected with the sampling channel assembly or the vacuum measuring assembly. The transition chamber is connected with a vacuum gauge and a vacuum transition pump set.
The vacuum measurement assembly comprises a mass spectrum chamber, a vacuum gauge, a mass spectrometer and a vacuum measurement pump set. The front end of the mass spectrum chamber directly acquires or is connected with the sampling channel assembly to acquire vacuum to be detected with certain air pressure. The mass spectrum chamber is connected with the vacuum gauge, the mass spectrometer and the vacuum measurement pump set.
In particular, a schematic structural diagram of a high-pressure gas sampling test apparatus according to an embodiment of the present application is shown in fig. 1.
As shown in FIG. 1, the high-pressure gas sampling test device comprises a vacuum transition assembly, a vacuum measurement assembly, a sampling channel assembly, a sample gas and data acquisition control system. The vacuum transition assembly and the vacuum measurement assembly each include a vacuum chamber. In this embodiment, the high-pressure gas to be measured sequentially passes through the vacuum transition assembly, the sampling channel assembly and the vacuum measurement assembly.
Specifically, as shown in fig. 1, the vacuum transition assembly includes a transition chamber 12, a vacuum gauge 32, an angle valve 48, a molecular pump 24, a three-way valve 47 and a mechanical pump 22, the vacuum transition assembly obtains the gas to be measured through a sampling pipeline, and the vacuum transition pump assembly is matched with the vacuum transition pump assembly to enable the collected high-pressure gas to be measured to be depressurized to a specific pressure according to requirements, and the vacuum transition pump assembly includes the molecular pump 24 and the mechanical pump 22.
The front end of the transition chamber is directly decompressed to obtain or is connected with the sampling channel assembly to obtain the high-pressure gas to be measured, and the rear end of the transition chamber is connected with the sampling channel assembly or the vacuum measuring assembly. In this embodiment, the transition chamber 12 is located at the front end of the sampling channel assembly, and high-pressure sample gas is introduced through the micro-adjustment valve 49 and the stop valve 410, the lower end of the transition chamber 12 is connected with the vacuum transition pump set, and the upper end of the transition chamber 12 is connected with the vacuum gauge 32.
Wherein, the vacuum transition pump group adopts a mechanical pump rough pumping mode and a molecular pump fine pumping mode, so that the ultimate vacuum of the transition chamber 12 is lower than 1 multiplied by 10 -3 Pa; by adjusting the front end trim valve 49 and the valve between the lower molecular pump 24 and the transition chamber 12, the valve includes an angle valve 48 and a three-way valve 47, a dynamically stable constant pressure gas flow can be established in the transition chamber. The transition chamber 12 is pressurized at 1 x 10 -3 Pa～10 5 And regulating the space between Pa, wherein the normal working vacuum is about 10 Pa. Transition chamber 12 is at 10Pa vacuumThe three sampling channels of the sampling channel assembly behind the chamber 12 and the air flow state in the mass spectrum chamber 11 of the vacuum measuring assembly are all in molecular flow state.
The transition chamber 12 decompresses the high-pressure gas to be detected to form the high-pressure gas to be detected with a certain pressure, and the rear end of the transition chamber 12 is connected with the sampling channel component. The sampling channel assembly includes at least one parallel sampling channel branch including a sampling channel and a shut-off valve. The shut-off valve of the sampling channel branch may be provided at one or both ends of the sampling channel.
As shown in fig. 1, in this embodiment, the sampling channel assembly includes three parallel sampling channel branches, where the sampling channel branches are respectively a small-hole sampling channel branch, a capillary sampling channel branch, and a sampling valve channel branch. Three parallel sampling channel branches are placed between the transition chamber 12 and the mass spectrometry chamber 11 of the vacuum measurement assembly for introducing a sample of the gas to be measured at a specific pressure formed in the transition chamber 12 onto a mass spectrometer 33 on the mass spectrometry chamber 11.
In this embodiment, the sampling channels of the three sampling channel branches are respectively a small-hole sampling channel, a capillary sampling channel and a sampling valve channel. The two ends of the small hole sampling channel, the capillary sampling channel and the sampling valve channel are all connected with the stop valve in a sealing way through quick connectors.
Specifically, after the pore sampling channel branch is connected with the transition chamber 12 of the vacuum transition assembly through the quick connector, the cut-off valve 46, the sampling pore 03 and the cut-off valve 43 are sequentially connected; the capillary sampling channel branch is connected with the transition chamber 12 of the vacuum transition assembly through a quick connector, and then is sequentially connected with a stop valve 45, a sampling capillary 02 and a stop valve 42; the sampling valve channel branch is connected with the transition chamber 12 of the vacuum transition assembly through a quick connector, and then is sequentially connected with the stop valve 44, the sampling valve 01 and the stop valve 41. The sampling channel component is connected in parallel through a plurality of sampling channel branches, and the mode of each channel branch is controlled through the stop valve respectively, so that on one hand, the on-off of one gas circuit is controlled independently without affecting other channels, and on the other hand, the sampling channel with other structures is replaced at any time according to requirements.
Specifically, the sampling valve 01, the sampling capillary vessel 02 and the sampling small holes 03 of the sampling channel can be detachably arranged on the branch of the sampling channel, the small hole size, the small hole number and the like of the sampling channel of the small holes can be replaced, the sampling channel of the capillary tube can be replaced by capillaries with other lengths, pipe diameters and materials, and the sampling valve channel can be an ALD sampling valve or a needle valve with different sizes and the like. And the three sampling channels can obtain the same conductance through adjustment.
And different sampling modes are selected through the sampling channel assembly, and the gas to be tested with specific pressure is sampled to the vacuum measurement assembly. The rear end of the sampling channel assembly is connected with a mass spectrum chamber 11 of the vacuum measuring assembly.
Specifically, as shown in fig. 1, the vacuum measurement assembly includes a mass spectrometry chamber 11, a vacuum gauge 31, a mass spectrometer 33, a molecular pump 23, and a mechanical pump 21. And after the vacuum measurement assembly is connected with the sampling channel assembly and matched with the vacuum measurement pump set to obtain the gas to be measured with specific pressure, the gas component analysis is carried out on the gas to be measured. The vacuum measurement pump set comprises a molecular pump 23 and a mechanical pump 21.
Specifically, the upper end of the mass spectrum chamber 11 is connected with the vacuum gauge 31, the lower end of the mass spectrum chamber 11 is connected with the molecular pump 23 and the mechanical pump 21, and the rear end of the mass spectrum chamber 11 is connected with the mass spectrometer 33.
Wherein, the vacuum measurement pump set adopts a mechanical dry pump rough pumping and a magnetic suspension molecular pump fine pumping mode to ensure that the ultimate vacuum of the mass spectrum chamber 11 is lower than 1 multiplied by 10 -7 Pa; the analyzer of the mass spectrometer 33 may be a quadrupole rod, and the ion source of the mass spectrometer 33 is a closed ion source, and the closed ion source may be directly connected with the rear end of the sampling channel in a sealing manner, so that the trace gas obtained by sampling in the sampling channel is directly sent into the mass spectrometer 33.
In the embodiment of the application, the valve is a numerical control electric valve, and the valve is controlled by computer operation, so that the sampling time can be conveniently recorded.
The sample gas is standard gas with known accurate calibration or concentration, and can be depressurized to 1 atmosphere by a pressure reducing valve.
The high-pressure gas sampling test device provided by the embodiment of the application further comprises a data acquisition control system, wherein the data acquisition control system is used for controlling the start and stop of the air pump group, the switch control of the vacuum valve, the switch control of the vacuum gauge and the switch control of the mass spectrometer 33. The data acquisition control system achieves the function of sampling and timing by controlling the switch of the vacuum valve.
The data acquisition control system also comprises a display module, wherein the display module is used for vacuum data acquisition display, mass spectrogram data acquisition display and sampling time display.
The high-pressure gas sampling test device based on the application can compare the influences of three sampling modes, namely a small hole sampling mode, a capillary sampling mode and a sampling valve mode, on sampling time and a component spectrogram. The method comprises the following steps:
step S1: the sampling structure with equal conductance after three sampling modes are calculated can be selected by selecting a proper sampling structure, three sampling channels are arranged between the transition chamber 12 and the mass spectrum chamber 11 in parallel, and meanwhile, the front end of the transition chamber 12 is connected with the sample gas through the fine tuning valve 49 and the stop valve 410.
Step S2: and determining standard sample injection gas, wherein a component spectrogram of the standard gas is required to be obtained before sample injection so as to compare the later results.
Step S3: after standard gas is introduced into the transition chamber 12 through the fine tuning valve 49 and the stop valve 410, the pressure of the transition chamber 12 is dynamically stabilized at 10Pa by adjusting the fine tuning valve 49 and valves between the transition chamber 12 and the molecular pump 24, so that the simulation of an extreme ultraviolet vacuum environment is facilitated, and the gas on a sampling channel can be in a molecular flow state.
Step S4: the mass spectrometer 33 on the mass spectrometry chamber 11 is turned on under a limiting vacuum while recording the ion flow of each mass number, i.e., the mass spectral composition spectrum, and the time profile of the gas composition of interest.
Step S5: opening a valve on any sampling channel branch, and starting timing; the mass spectrum change and the gas composition change of the mass spectrometer 33 with time are observed until a stable mass spectrum is sampled, and the timing is finished, and the mass spectrum, the transition chamber 12 and the mass spectrum chamber 11 vacuum pressures are recorded.
Step S6: and after the end, the sampling channel is blocked by a stop valve of the corresponding channel branch.
Step S7: and sequentially opening the stop valves of the other two sampling channels, and repeating the step S5, so that mass spectrograms, sampling time and chamber pressure before and after sampling of three different sampling modes under the molecular flow state are obtained.
Step S8: and comparing mass spectrograms, sampling time and chamber pressure before and after sampling of the three sampling modes under the molecular flow state, and simultaneously comparing the mass spectrograms with a standard component spectrogram of standard gas to obtain the optimal sampling mode.
As other embodiments, if it is necessary to explore the influence of factors such as the length of the capillary, the diameter of the capillary, the capillary material, the size of the small holes, and the number of the small holes on the analysis result of the gas component, the sampling channel can be disassembled to be replaced, the sampling structure is modified, and then the step S5 is repeated, so that mass spectrograms, sampling time and chamber pressures before and after sampling under different molecular flow states of the sampling structure can be obtained. And finally comparing the two components with each other and comparing the two components with a standard component spectrogram to obtain an optimal sampling structure and an optimal sampling mode.
In this embodiment, the sampling channel assembly is detachably mounted. The fine adjustment valve 49 and the shut-off valve 410 are also detachably attached. Thus, based on the embodiment of the high-pressure gas sampling test apparatus shown in fig. 1, other configurations of the high-pressure gas sampling test apparatus may be formed as required for the test.
A schematic structural diagram of a high pressure gas sampling test apparatus according to another embodiment of the present application is shown in fig. 2. As shown in fig. 2, a trim valve 49 and a shut-off valve 410 are placed between the transition chamber 12 and the mass spectrometry chamber 11, while three parallel sampling channels are placed between the front end of the transition chamber 12 and the sample gas. The sampling channel component is used for collecting high-pressure gas to be tested to the vacuum transition component. The sampling test device in the mode is used for sampling viscous flow, and the applicability of different sampling modes under different flow states is obtained by replacing the positions of the components.
In practice, the trim valve 49 and the shut-off valve 410 are placed between the transition chamber 12 and the mass spectrometry chamber 11, while three parallel sampling channels are placed between the front end of the transition chamber 12 and the sample gas. For comparison of different sampling patterns under viscous flow, and then obtaining the applicability of the gas sampling pattern under the gas flow state. Similarly, if the influence of factors such as capillary length, capillary diameter, capillary material, pore size and pore number on the analysis result of the gas component is required to be explored, the sampling channel can be disassembled for replacement, and after the sampling structure is modified, mass spectrograms, sampling time and chamber pressure before and after sampling under different viscous flow states of the sampling structure are obtained. And finally comparing the two components with each other and comparing the two components with a standard component spectrogram to obtain an optimal sampling structure and a sampling mode under the flow state.
A schematic structural diagram of a high pressure gas sampling test apparatus according to another embodiment of the present application is shown in fig. 3. As shown in fig. 3, the vacuum transition assembly and sampling channel assembly can be removed directly, connecting the trim valve 49 and shut-off valve 410 directly to the mass spectrometry chamber 11. By the sampling device, high-pressure gas to be detected can be directly sampled into a closed ion source of the mass spectrometer. The influence of the direct analysis and comparison micro-adjustment valve on the analysis result of the gas component can be realized.
In specific implementation, the high-pressure gas to be detected is directly connected with the mass spectrum chamber 11 through the fine tuning valve and the stop valve, and the sample gas can be directly sampled into the closed ion source of the mass spectrometer through the high-precision adjustment of the fine tuning valve 49, so that the influence of the fine tuning valve 49 on the mass spectrogram and the sampling time is directly compared. Thus, when the influence of the up-sampling mode on the sampling result is analyzed, the sampling influence of the fine adjustment valve 49 can be removed, and the analysis result is more accurate.
Fig. 4 shows a schematic structural diagram of a high-pressure gas sampling test apparatus according to another embodiment of the present application. As shown in fig. 4, the trim valve 49 and the shut-off valve 410 are removed and three suitable sampling channels of the sampling channel assembly are provided at each end of the transition chamber 12. The sampling channel assembly is used for sampling the high-pressure gas to be measured to the vacuum transition assembly and sampling the gas to be measured with the specific pressure of the vacuum transition assembly to the vacuum measurement assembly respectively. The sampling test device can realize the combination of two different sampling modes, and comprehensively compare the influence of the sampling test device on the analysis result of the gas components.
In the embodiment of the high-pressure gas sampling test apparatus shown in fig. 4, the two selected sampling modes can be comprehensively compared by using a cross test method to influence the analysis result of the gas component. The two sampling modes can be comprehensively compared with each other by adopting a cross test method, and the cross test method is designed as shown in the following table 1.
| Influencing factors | Small hole A 2 | Capillary B 2 | Sampling valve C 2 |
| Small hole A 1 | A 1 A 2 | A 1 B 2 | A 1 C 2 |
| Capillary B 1 | B 1 A 2 | B 1 B 2 | B 1 C 2 |
| Sampling valve C 1 | C 1 A 2 | C 1 B 2 | C 1 C 2 |
TABLE 1 Cross test method for high pressure gas sampling
By adopting the high-pressure gas sampling test device in the embodiment of the application, the atmosphere with stable concentration can be conveniently obtained as standard sample gas, and the needle valve and the capillary tube are respectively adopted for sampling under the viscous flow state, so that the working vacuum of the transition chamber is stabilized at 150Pa, and the working vacuum of the mass spectrum chamber is stabilized at 5 multiplied by 10 -4 Pa。
First, the atmospheric spectrograms under two sampling modes are measured, and fig. 5 shows a comparison chart of the atmospheric spectrograms obtained by sampling a needle Valve (Valve) and a capillary (capillary) according to an embodiment of the present application. As shown in fig. 5, it can be seen that the atmospheric spectra obtained by needle Valve (Valve) sampling and capillary (capillary) sampling are almost identical, and the peak shapes are also identical. The response time of the needle valve sampling atmosphere is 3-5 s, and the needle valve sampling atmosphere almost responds instantaneously; the response time of the capillary sampling atmosphere is 10-15 s, namely the capillary sampling has the problem of delayed response.
Further, since xenon is the least one of the rare gases in the air and the content is relatively stable, the isotope content spectrum of trace xenon in the air is sampled and analyzed, and fig. 6 shows a comparison graph of isotope spectra of trace xenon in the atmosphere obtained by needle Valve (Valve) and capillary (capillary) sampling according to the embodiment of the present application. As shown in fig. 6, it can be seen that the needle sampling obtained xenon each isotope ion number is smaller than that obtained by capillary sampling, and at the same time, the needle sampling mass spectrum peak shape is inferior to that of capillary sampling. The structure combining the two sampling modes can analyze specific reasons.
The high-pressure gas sampling test device comprises a vacuum transition assembly, a vacuum measurement assembly and a sampling channel assembly; the vacuum transition assembly is used for decompressing and acquiring high-pressure gas to be detected with certain air pressure; the vacuum measurement assembly is used for measuring the gas composition of the high-pressure gas to be measured; the sampling channel component is used for connecting the vacuum transition component and/or the vacuum measurement component; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch. The high-pressure gas sampling test device and the sampling test method can systematically study and analyze the influence of one or more gas sampling modes on gas component analysis.
The sampling mode provided by the high-pressure gas sampling test device provided by the embodiment of the application is used for exploring gas, analyzing the influence of the sampling mode on gas component analysis, and comparing the sampling time length and component spectrogram of the same standard gas source through capillary sampling, small hole sampling and valve sampling; the influence of the length, the diameter, the material, the size and the number of the small holes of the capillary on the analysis result of the gas component can be explored; and the sampling results of the sampling modes can be compared under different gas flow states by replacing the positions of the components, and finally, the applicability analysis of the sampling modes is carried out.
Example 2
The present embodiment provides a high-pressure gas sampling test method, and for details not disclosed in the high-pressure gas sampling test method of the present embodiment, please refer to the high-pressure gas sampling test device in other embodiments.
Fig. 7 shows a flow chart of steps of a high pressure gas sampling test method according to an embodiment of the present application.
As shown in fig. 7, the high-pressure gas sampling test method specifically includes the following steps:
step S10: and decompressing to obtain the high-pressure gas to be detected with certain air pressure.
And acquiring high-pressure gas to be detected through the vacuum transition assembly, and then reducing the pressure of the acquired high-pressure gas to be detected to a certain pressure according with the requirement under the action of the vacuum transition pump group to form the high-pressure gas to be detected with a certain pressure.
Step S20: and indirectly measuring the gas composition of the high-pressure gas to be measured.
And after the vacuum measurement assembly is matched with the vacuum measurement pump set to obtain the gas to be measured with specific pressure, carrying out gas component analysis on the gas to be measured through the mass spectrometer.
In both step S10 and step S20, gas sampling methods may be selected when gas is acquired, so that the sampling method may be selected when the gas to be measured is sampled and acquired before step S10, or the sampling method may be selected when the gas to be measured with a certain pressure formed by decompression is sampled and acquired after step S10.
The sampling mode is selected as step S30, and step S30 is used for obtaining high-pressure gas to be detected through decompression of the sampling channel component and/or obtaining high-pressure gas to be detected with certain air pressure through the sampling channel component. Wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch.
The method for sampling and testing the high-pressure gas based on the application can compare the influences of three sampling modes, namely a small-hole sampling mode, a capillary sampling mode and a sampling valve mode, on sampling time and a component spectrogram. The method comprises the following steps:
step S1: as shown in fig. 1, a suitable sampling structure is selected, and a sampling structure with equal conductance after three sampling modes are calculated is selected, three sampling channels are arranged in parallel between the transition chamber 12 and the mass spectrum chamber 11, and meanwhile, the front end of the transition chamber 12 is connected with sample gas through a fine tuning valve 49 and a stop valve 410.
Step S2: and determining standard sample injection gas, wherein a component spectrogram of the standard gas is required to be obtained before sample injection so as to compare the later results.
Step S3: after standard gas is introduced into the transition chamber 12 through the fine tuning valve 49 and the stop valve 410, the pressure of the transition chamber 23 is dynamically stabilized at 10Pa by adjusting the fine tuning valve 49 and valves between the transition chamber 12 and the molecular pump 24, so that the simulation of an extreme ultraviolet vacuum environment is facilitated, and the gas on a sampling channel can be in a molecular flow state.
Step S4: the mass spectrometer 33 on the mass spectrometry chamber 11 is turned on under a limiting vacuum while recording the ion flow of each mass number, i.e., the mass spectral composition spectrum, and the time profile of the gas composition of interest.
Step S5: opening a valve on any sampling channel branch, and starting timing; the mass spectrum change and the gas composition change of the mass spectrometer 33 with time are observed until a stable mass spectrum is sampled, and the timing is finished, and the mass spectrum, the transition chamber 12 and the mass spectrum chamber 11 vacuum pressures are recorded.
Step S6: and after the end, the sampling channel is blocked by a stop valve of the corresponding channel branch.
Step S7: and sequentially opening the stop valves of the other two sampling channels, and repeating the step S5, so that mass spectrograms, sampling time and chamber pressure before and after sampling of three different sampling modes under the molecular flow state are obtained.
Step S8: and comparing mass spectrograms, sampling time and chamber pressure before and after sampling of the three sampling modes under the molecular flow state, and simultaneously comparing the mass spectrograms with a standard component spectrogram of standard gas to obtain the optimal sampling mode.
As other embodiments, if it is necessary to explore the influence of factors such as the length of the capillary, the diameter of the capillary, the capillary material, the size of the small holes, and the number of the small holes on the analysis result of the gas component, the sampling channel can be disassembled to be replaced, the sampling structure is modified, and then the step S5 is repeated, so that mass spectrograms, sampling time and chamber pressures before and after sampling under different molecular flow states of the sampling structure can be obtained. And finally comparing the two components with each other and comparing the two components with a standard component spectrogram to obtain an optimal sampling structure and an optimal sampling mode.
In this embodiment, the sampling channel assembly is detachably mounted. The fine adjustment valve 49 and the shut-off valve 410 are also detachably attached. Thus, based on the embodiment of the high-pressure gas sampling test apparatus shown in fig. 1, other configurations of the high-pressure gas sampling test apparatus may be formed as required for the test.
In another embodiment of the high pressure gas sampling test method, as shown in fig. 2, a micro-tuning valve 49 and a stop valve 410 are placed between the transition chamber 12 and the mass spectrometry chamber 11, and three parallel sampling channels are placed between the front end of the transition chamber 12 and the sample gas. The sampling channel component is used for collecting high-pressure gas to be tested to the vacuum transition component. The sampling test device in the mode is used for sampling viscous flow, and the applicability of different sampling modes under different flow states is obtained by replacing the positions of the components.
In practice, the trim valve 49 and the shut-off valve 410 are placed between the transition chamber 12 and the mass spectrometry chamber 11, while three parallel sampling channels are placed between the front end of the transition chamber 12 and the sample gas. For comparison of different sampling patterns under viscous flow, and then obtaining the applicability of the gas sampling pattern under the gas flow state. Similarly, if the influence of factors such as capillary length, capillary diameter, capillary material, pore size and pore number on the analysis result of the gas component is required to be explored, the sampling channel can be disassembled for replacement, and after the sampling structure is modified, mass spectrograms, sampling time and chamber pressure before and after sampling under different viscous flow states of the sampling structure are obtained. And finally comparing the two components with each other and comparing the two components with a standard component spectrogram to obtain an optimal sampling structure and an optimal sampling mode.
In another embodiment of the high pressure gas sampling test method, as shown in fig. 3, the vacuum transition assembly and the sampling channel assembly can be removed directly, and the trim valve 49 and the shut-off valve 410 can be connected directly to the mass spectrometry chamber 11. By the sampling test device, high-pressure gas to be tested can be directly sampled into a closed ion source of the mass spectrometer. The influence of the direct analysis and comparison micro-adjustment valve on the analysis result of the gas component can be realized.
In specific implementation, the gas to be detected is directly connected with the mass spectrum chamber 11 through the fine tuning valve and the stop valve, and the sample gas can be directly sampled into the closed ion source of the mass spectrometer through the high-precision adjustment of the fine tuning valve 49, so that the influence of the fine tuning valve 49 on the mass spectrogram and the sampling time can be directly compared. Thus, when the influence of the up-sampling mode on the sampling result is analyzed, the sampling influence of the fine adjustment valve 49 can be removed, and the analysis result is more accurate.
In another embodiment of the high pressure gas sampling test method, as shown in fig. 4, the trimming valve 49 and the stop valve 410 are removed, and three suitable sampling channels of the sampling channel assembly are respectively disposed at two ends of the transition chamber 12. The sampling channel assembly is used for collecting the gas to be measured to the vacuum transition assembly and collecting the gas to be measured with specific pressure of the vacuum transition assembly to the vacuum measurement assembly respectively. The sampling test device can realize the combination of two different sampling modes, and comprehensively analyze the influence of the sampling modes on the analysis result of the gas component.
The two sampling modes selected by the cross test method are comprehensively compared and influence on the analysis result of the gas component is combined. The effect of the combination of the two sampling modes on the analysis result of the gas component can be comprehensively compared by adopting a cross test method, and the design of the cross test method is shown in the following table 1.
| Influencing factors | Small hole A 2 | Capillary B 2 | Sampling valve C 2 |
| Small hole A 1 | A 1 A 2 | A 1 B 2 | A 1 C 2 |
| Capillary B 1 | B 1 A 2 | B 1 B 2 | B 1 C 2 |
| Sampling valve C 1 | C 1 A 2 | C 1 B 2 | C 1 C 2 |
TABLE 1 Cross test method for high pressure gas sampling
By adopting the high-pressure gas sampling test method in the embodiment of the application, the atmosphere with stable concentration can be conveniently obtained as standard sample gas, and the needle valve and the capillary tube are respectively adopted for sampling under the viscous flow state, so that the working vacuum of the transition chamber is stabilized at 150Pa, and the working vacuum of the mass spectrum chamber is stabilized at 5 multiplied by 10 -4 Pa。
First, the atmospheric spectrograms under two sampling modes are measured, and fig. 5 shows a comparison chart of the atmospheric spectrograms obtained by sampling a needle Valve (Valve) and a capillary (capillary) according to an embodiment of the present application. As shown in fig. 5, it can be seen that the atmospheric spectra obtained by needle Valve (Valve) sampling and capillary (capillary) sampling are almost identical, and the peak shapes are also identical. The response time of the needle valve sampling atmosphere is 3-5 s, and the needle valve sampling atmosphere almost responds instantaneously; the response time of the capillary sampling atmosphere is 10-15 s, namely the capillary sampling has the problem of delayed response.
Further, since xenon is the least one of the rare gases in the air and the content is relatively stable, the isotope content spectrum of trace xenon in the air is sampled and analyzed, and fig. 6 shows a comparison graph of isotope spectra of trace xenon in the atmosphere obtained by needle Valve (Valve) and capillary (capillary) sampling according to the embodiment of the present application. As shown in fig. 6, it can be seen that the needle sampling obtained xenon each isotope ion number is smaller than that obtained by capillary sampling, and at the same time, the needle sampling mass spectrum peak shape is inferior to that of capillary sampling. The structure combining the two sampling modes can analyze specific reasons.
By adopting the high-pressure gas sampling test method in the embodiment of the application, firstly, the high-pressure gas to be tested with certain air pressure is obtained by decompression; secondly, indirectly measuring the gas composition of the high-pressure gas to be measured; then, the high-pressure gas to be detected is obtained through the sampling channel assembly in a decompression mode, and/or the gas to be detected with certain air pressure is obtained through the sampling channel assembly; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch. The influence of a certain or a plurality of gas sampling modes on the analysis of the gas components can be systematically researched and analyzed by the high-pressure gas sampling test method.
The sampling test method is used for exploring gas, analyzing the research of the influence of a sampling mode on the analysis of gas components, and comparing the sampling duration and component spectrograms of the same standard gas source through capillary sampling, small hole sampling and valve sampling; the influence of the length, the diameter, the material, the size and the number of the small holes of the capillary on the analysis result of the gas component can be explored; and the sampling results of the sampling modes can be compared under different gas flow states by replacing the positions of the components, and finally, the applicability analysis of the sampling modes is carried out.
While preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present application without departing from the spirit or scope of the application. Thus, if such modifications and variations of the present application fall within the scope of the claims and the equivalents thereof, the present application is intended to cover such modifications and variations.
Claims (10)
1. A high pressure gas sampling test apparatus, comprising:
the vacuum transition assembly is used for decompressing and acquiring high-pressure gas to be detected with certain air pressure;
the vacuum measurement assembly is used for measuring the gas composition of the high-pressure gas to be measured;
the sampling channel assembly is used for connecting the vacuum transition assembly and/or the vacuum measurement assembly; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch;
the sampling valve, the sampling capillary and the sampling small holes of the sampling channel are detachably arranged on the sampling channel branch, the small hole size and the small hole number of the small hole sampling channel can be replaced, the capillary sampling channel can be replaced by capillaries with other lengths, pipe diameters and materials, and the sampling valve channel can be an ALD sampling valve or needle valve with different sizes; the three sampling channels can obtain the same conductance through adjustment;
when molecular flow state sampling is carried out, the sampling channel component is arranged behind the vacuum excessive component along the gas flow direction, and when viscous flow sampling is carried out, the sampling channel component is arranged in front of the vacuum excessive component along the gas flow direction.
2. The high pressure gas sampling test apparatus of claim 1, wherein the vacuum transition assembly comprises a transition chamber, a vacuum gauge, and a vacuum transition pump stack; the front end of the transition chamber is directly decompressed to obtain or is connected with the sampling channel assembly to obtain high-pressure gas to be tested, and the rear end of the transition chamber is connected with the sampling channel assembly or the vacuum measuring assembly; the transition chamber is connected with a vacuum gauge and a vacuum transition pump set.
3. The high pressure gas sampling test apparatus of claim 1, wherein the vacuum measurement assembly comprises a mass spectrometry chamber, a vacuum gauge, a mass spectrometer, and a vacuum measurement pump set; the front end of the mass spectrum chamber is directly acquired or connected with the sampling channel assembly to acquire vacuum to be measured with certain air pressure, and the mass spectrum chamber is connected with a vacuum gauge, a mass spectrometer and a vacuum measurement pump set.
4. The high pressure gas sampling test apparatus of claim 1, wherein the vacuum transition assembly and the vacuum measurement assembly each comprise a molecular pump and a mechanical pump.
5. The high pressure gas sampling test apparatus of claim 1, wherein the sampling channel branch comprises a sampling channel and a shut-off valve.
6. The high-pressure gas sampling test apparatus according to claim 5, wherein the shutoff valve of the sampling passage branch is provided at one end or both ends of the sampling passage.
7. The high pressure gas sampling test apparatus of claim 5, wherein the sampling passage is removably mounted to the sampling passage branch.
8. The high-pressure gas sampling test apparatus according to claim 1, further comprising a fine tuning valve disposed on a passage between the vacuum measuring assembly and the vacuum transition assembly or on a passage through which the vacuum transition assembly decompresses to obtain the high-pressure gas to be measured.
9. The high-pressure gas sampling test method is characterized by comprising the following steps of:
decompressing to obtain high-pressure gas to be detected with certain air pressure;
measuring the gas composition of the high-pressure gas to be measured;
obtaining high-pressure gas to be detected through a sampling channel assembly, and/or obtaining the high-pressure gas to be detected with certain air pressure through the sampling channel assembly; wherein the sampling channel assembly comprises at least two of the following sampling channel branches in parallel: a small hole sampling channel branch, a capillary sampling channel branch and a sampling valve channel branch;
the sampling valve, the sampling capillary and the sampling small holes of the sampling channel are detachably arranged on the sampling channel branch, the small hole size and the small hole number of the small hole sampling channel can be replaced, the capillary sampling channel can be replaced by capillaries with other lengths, pipe diameters and materials, and the sampling valve channel can be an ALD sampling valve or needle valve with different sizes; the three sampling channels can obtain the same conductance through adjustment;
when molecular flow state sampling is carried out, the sampling channel component is arranged behind the vacuum excessive component along the gas flow direction, and when viscous flow sampling is carried out, the sampling channel component is arranged in front of the vacuum excessive component along the gas flow direction.
10. The high pressure gas sampling test method of claim 9, wherein the sampling channel branch comprises a sampling channel and a shut-off valve.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008095504A (en) * | 2006-10-05 | 2008-04-24 | Agilent Technol Inc | Analysis apparatus |
| CN205720136U (en) * | 2016-03-23 | 2016-11-23 | 中国科学院光电研究院 | A kind of online process gas sampling and analyzing device |
| CN206362660U (en) * | 2016-12-08 | 2017-07-28 | 中国科学院光电研究院 | A kind of material radiation causes the online testing device deflated |
| CN107356458A (en) * | 2017-06-27 | 2017-11-17 | 爱文思控制系统工程(上海)有限公司 | A kind of online air detection sample drying and control system |
| CN208208713U (en) * | 2018-06-19 | 2018-12-07 | 中国科学院光电研究院 | A kind of detection device of high-precision mass spectrum detection limit |
| CN109459192A (en) * | 2018-12-06 | 2019-03-12 | 北京东方计量测试研究所 | A kind of molecular flow sampling system and control method based on comparison method calibration positive pressure leak hole |
| CN110376272A (en) * | 2019-06-12 | 2019-10-25 | 中国科学院微电子研究所 | The on-line measurement device and its On-line Measuring Method of partial pressure |
-
2020
- 2020-05-13 CN CN202010404156.1A patent/CN111665292B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008095504A (en) * | 2006-10-05 | 2008-04-24 | Agilent Technol Inc | Analysis apparatus |
| CN205720136U (en) * | 2016-03-23 | 2016-11-23 | 中国科学院光电研究院 | A kind of online process gas sampling and analyzing device |
| CN206362660U (en) * | 2016-12-08 | 2017-07-28 | 中国科学院光电研究院 | A kind of material radiation causes the online testing device deflated |
| CN107356458A (en) * | 2017-06-27 | 2017-11-17 | 爱文思控制系统工程(上海)有限公司 | A kind of online air detection sample drying and control system |
| CN208208713U (en) * | 2018-06-19 | 2018-12-07 | 中国科学院光电研究院 | A kind of detection device of high-precision mass spectrum detection limit |
| CN109459192A (en) * | 2018-12-06 | 2019-03-12 | 北京东方计量测试研究所 | A kind of molecular flow sampling system and control method based on comparison method calibration positive pressure leak hole |
| CN110376272A (en) * | 2019-06-12 | 2019-10-25 | 中国科学院微电子研究所 | The on-line measurement device and its On-line Measuring Method of partial pressure |
Non-Patent Citations (1)
| Title |
|---|
| 罗艳 ; 王魁波 ; 吴晓斌 ; 王宇 ; .超高精度质谱检出限的测试技术研究.真空科学与技术学报.2018,第38卷(第11期),全文. * |
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