CN111638263A - Gas sampling and analyzing device and method - Google Patents

Abstract

The invention discloses a gas sampling and analysis device and method, the device comprises: a vacuum acquisition module, a sampling module and a gas analysis module; wherein, the gas analysis module is respectively connected with the vacuum acquisition module and the sampling module; wherein , the vacuum acquisition module includes a restrictor valve, and when the restrictor valve is opened and closed, the ultimate vacuum and the working vacuum of the gas analysis module are respectively realized. Therefore, by adopting the embodiments of the present application, it is possible to perform on-line analysis of high-pressure, normal-pressure and vacuum gases; increase the gas sampling amount, improve the system response speed; eliminate the molecular discrimination effect and pumping speed selectivity during gas sampling, and realize non-destructive sampling Analyze and realize the calibration of the gas sampling and analysis device, so as to improve the accuracy of the gas sampling and analysis results.

Description

A kind of gas sampling analysis device and method

technical field

The invention relates to the technical field of measurement, in particular to a gas sampling and analysis device and method, which can be used for sampling and component analysis of high-pressure, normal-pressure and vacuum gases.

Background technique

In the field of industrial production, it is often necessary to analyze the gas composition, partial pressure and concentration of various process chambers to determine whether the gas content is within a reasonable range, and timely feedback control to ensure the normal operation of industrial production. For example: in the synthesis of urea, the ratio of ammonia and carbon dioxide in the synthesis tower needs to be kept within a certain range, and the concentration of ammonia and carbon dioxide needs to be analyzed for this purpose. This reaction process is usually carried out in a high pressure environment, such as above 150 atmospheres. For another example, gas lasers are widely used in industry, and their working fluids are often mixed gases. The working pressure of the working medium is wide, such as 2 to 6 atmospheres. The performance of the gas laser is closely related to the composition and concentration of the working fluid gas, as well as the content of the polluting gas in the working fluid. It is necessary to analyze the gas composition and concentration in the discharge cavity of the gas laser in real time. For another example, the vacuum system of the extreme ultraviolet (EUV) lithography machine contains many process chambers with different requirements, and the gas content in each vacuum chamber needs to be closely monitored at all times, such as the composition and partial pressure of gases such as H2O, O2, and CxHy. . Common sampling methods are: volume sampling method, sampling valve, pipeline, micropore and membrane sampling, etc. The partial pressure ratio will change during the transmission of the mixed gas from the high pressure end to the low pressure end, so that the actual measured gas composition is different from the gas composition. The composition of the gas source in the process chamber is different, and even part of the trace gas is lost, which reduces the accuracy of the gas analysis.

SUMMARY OF THE INVENTION

The embodiments of the present application provide a gas sampling and analysis device and method. In order to provide a basic understanding of some aspects of the disclosed embodiments, a brief summary is given below. This summary is not intended to be an extensive review, nor is it intended to identify key/critical elements or delineate the scope of protection of these embodiments. Its sole purpose is to present some concepts in a simplified form as a prelude to the detailed description that follows.

In a first aspect, an embodiment of the present application provides a gas sampling and analysis device, the device comprising:

vacuum acquisition module, sampling module and gas analysis module; wherein,

The gas analysis module is respectively connected with the vacuum acquisition module and the sampling module; wherein,

The vacuum acquisition module includes a restrictor valve, and when the restrictor valve is opened and closed, the ultimate vacuum and the working vacuum of the gas analysis module are respectively realized; wherein,

The restrictor valve is a vacuum valve with a through hole of a suitable size on the valve plate.

Optionally, the device further includes:

A calibration module; wherein, the calibration module is connected with the sampling module.

Optionally, the vacuum acquisition module includes a restrictor valve, a main pump, a solenoid valve, and a fore pump; the restrictor valve, the main pump, the electromagnetic valve, and the fore pump are sequentially connected through a pipeline; the current restrictor One end of the valve is connected to the main pump through the pipeline, and the other end is connected to the gas analysis module through the pipeline; wherein, the requirements for the size of the opening on the valve plate of the restrictor valve include at least: 1. The size of the opening corresponds to The molecular flow pumping speed can meet the needs of working vacuum pumping in the analysis room. ② The molecular flow pumping speed corresponding to the opening size should not exceed 25% of the pumping speed of the main pump.

Optionally, the sampling module includes a process chamber, a valve group, a first regulating valve and a flow restrictor; wherein, the process chamber, the valve group and the flow restrictor are sequentially connected through a sampling pipe, one end of the sampling pipe Inserted into the process chamber, the other end is connected to one end of the valve group; the other end of the valve group is connected to one end of the flow restrictor through the sampling pipe; the other end of the flow restrictor passes through the sampling pipe The pipe is connected to the gas analysis module; one end of the first regulating valve is connected to the valve group and the sampling pipe connected to the flow restrictor through a pipeline, and the other end of the first regulating valve is connected to the pipeline to the vacuum acquisition module. Optionally, the gas analysis module includes an analysis chamber, a vacuum gauge and a gas analyzer, and the analysis chamber is respectively connected to the vacuum gauge and the gas analyzer through pipes; wherein,

The analysis chamber can also be respectively connected to the vacuum gauge and the gas analyzer through a valve;

Wherein, the gas analysis module can select at least a quadrupole mass spectrometer, a time-of-flight mass spectrometer, and an ion trap mass spectrometer; wherein;

A heater is arranged on the pipeline and the analysis chamber, and the heater can bake and degas the sampling pipeline and the analysis chamber.

Optionally, the calibration module includes a standard gas source and a second regulating valve, the standard gas source is connected to one end of the second regulating valve through a pipeline, and the other end of the second regulating valve is connected to the valve group through a pipeline , and the sampling pipe connected to the flow restrictor; wherein, the standard gas source can provide high-purity standard gas for the gas analysis device, and the standard gas is a mixture of multiple gases with a certain concentration.

Optionally, the sampling module includes a process chamber, a valve group, a first regulating valve, a vacuum pump and a flow restrictor; wherein, the process chamber, the valve group and the flow restrictor are connected in sequence through a sampling pipe, and the sampling One end of the pipe is inserted into the interior of the process chamber, and the other end is connected to one end of the valve group; the other end of the valve group is connected to one end of the flow restrictor through the sampling pipe; the other end of the flow restrictor passes through the The sampling pipe is connected to the gas analysis module; one end of the first regulating valve is connected to the valve group and the sampling pipe connected to the flow restrictor through a pipeline, and the other end of the first regulating valve is The tubing is connected to the vacuum pump. Wherein, the flow restrictor adopts at least a capillary tube, a micropore and a fine adjustment valve, and the capillary tube or the micropore is preferably used.

Optionally, when the high-pressure or normal-pressure gas is in the process chamber, continuous flow sampling is used; when the process chamber is in a vacuum environment, molecular flow sampling is used. Correspondingly, the relationship between the diameter of the sampling tube and the free path of gas molecules passing through the sampling tube are:

d≥10λ(1)

d≤λ/10(2)

Wherein, d is the diameter of the sampling tube, and λ is the free path of gas molecules.

Optionally, the vacuum acquisition module is used for evacuating the analysis chamber; the sampling module is used for the analysis chamber to acquire the gas to be detected; the gas analysis module is used for the gas to be detected in the analysis chamber. performing detection and analysis; the calibration module is used to periodically calibrate the gas sampling and analysis device.

In a second aspect, an embodiment of the present application provides a gas sampling and analysis method, the method comprising:

Close the valve group, the first regulating valve and the second regulating valve, and turn on the vacuum gauge, the backing pump, the solenoid valve, the main pump and the restrictor valve to pump the ultimate vacuum to the analysis chamber;

When the vacuum degree of the analysis chamber reaches the preset threshold, turn on the gas analysis module to monitor the analysis chamber in real time;

When no polluting gas is detected by the gas analysis module, the gas analysis module and the restrictor valve are closed, the valve group is opened, and the first regulating valve is adjusted until the analysis chamber obtains a working vacuum, and then the gas analysis module is opened to analyze and test the sampled gas;

Close the valve group and the first regulating valve, open the restrictor valve and continue to pump the ultimate vacuum to the device;

When no polluting gas is detected by the gas analysis module, turn off the gas sampling and analysis device and keep it in a vacuum state.

The technical solutions provided by the embodiments of the present application may include the following beneficial effects:

The advantages of this application are: (1) online analysis of high pressure, normal pressure and vacuum gases, (2) increased gas sampling volume and improved system response speed, (3) elimination of molecular discrimination effect and pumping speed selection during gas sampling properties, so as to achieve non-destructive sampling analysis, (4) automatic calibration.

It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention.

Description of drawings

The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description serve to explain the principles of the invention.

1 is a schematic diagram of a gas sampling and analysis device provided in an embodiment of the present application;

2 is a schematic diagram of another gas sampling and analysis device provided in an embodiment of the present application;

3 is a schematic flowchart of a gas sampling and analysis method provided by an embodiment of the present application;

4 is a schematic process diagram of a gas sampling analysis process provided by an embodiment of the present application;

Detailed ways

The following description and drawings sufficiently illustrate specific embodiments of the invention to enable those skilled in the art to practice them.

It should be understood that the described embodiments are only some, but not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

Where the following description refers to the drawings, the same numerals in different drawings refer to the same or similar elements unless otherwise indicated. The implementations described in the illustrative examples below are not intended to represent all implementations consistent with the present invention. Rather, they are merely examples of apparatus and methods consistent with some aspects of the invention, as recited in the appended claims.

In the description of the present invention, it should be understood that the terms "first", "second" and the like are used for descriptive purposes only, and should not be construed as indicating or implying relative importance. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood in specific situations. Furthermore, in the description of the present invention, unless otherwise specified, "a plurality" means two or more. "And/or", which describes the association relationship of the associated objects, means that there can be three kinds of relationships, for example, A and/or B, which can mean that A exists alone, A and B exist at the same time, and B exists alone. The character "/" generally indicates that the associated objects are an "or" relationship.

So far, the common sampling methods for gas sampling and analysis are: volume sampling method, sampling valve, pipeline, micropore and membrane sampling, etc. The partial pressure ratio will change during the transmission of mixed gas from the high pressure end to the low pressure end. The actual measured gas composition is different from the gas source composition in the process chamber, and even part of the trace gas is lost, thereby reducing the accuracy of gas analysis. To this end, the present application provides a gas sampling and analysis device and method to solve the problems existing in the above-mentioned related technical problems. In the technical solution provided in this application, the valve group, the first regulating valve and the second regulating valve are closed, and the vacuum gauge, the backing pump, the solenoid valve, the main pump and the restrictor valve are turned on to pump the ultimate vacuum to the analysis chamber; When the vacuum degree of the chamber reaches the preset threshold, open the gas analysis module to monitor the analysis chamber in real time; when the gas analysis module does not detect polluting gas, close the gas analysis module and the restrictor valve, open the valve group and adjust the first Adjust the valve until the working vacuum is obtained in the analysis chamber, and then open the gas analysis module to analyze and test the sampled gas; close the valve group and the first regulating valve, and open the limiting valve to continue to pump the ultimate vacuum to the device; when the gas analysis module does not detect any polluting gas At this time, the gas sampling and analysis device is turned off to keep it in a vacuum state, so as to improve the accuracy of gas sampling and analysis, which will be described in detail below using an exemplary embodiment.

Please refer to FIG. 1. FIG. 1 is a schematic diagram of a gas sampling and analysis device provided in an embodiment of the present application. The device includes a vacuum acquisition module, a sampling module, a gas analysis module, and a calibration module, wherein the vacuum acquisition module includes a restrictor valve 8. , the main pump 9, the solenoid valve 10 and the fore pump 11, wherein the restrictor valve 8, the main pump 9, the solenoid valve 10 and the fore pump 11 are connected in turn through the pipeline, and one end of the restrictor valve 8 is connected to the main pump through the pipeline. The other end of the pump 9 is connected to the gas analysis module through a pipeline. The sampling module includes a process chamber, a valve group, a first regulating valve and a flow restrictor, wherein the process chamber 1, the valve group 3 and the flow restrictor 4 are connected in sequence through a sampling pipe 2, and one end of the sampling pipe 2 is inserted into the interior of the process chamber 1 , the other end is connected to one end of the valve group 3, the other end of the valve group 3 is connected to one end of the restrictor 4 through the sampling pipe 2, and the other end of the restrictor 4 is connected to the gas analysis module through the sampling pipe; one end of the first regulating valve 12 The valve block 3 is connected to the sampling pipe connected to the restrictor 4 through a pipeline, and the other end of the first regulating valve 12 is connected to the backing pump 11 and the pipeline connected to the solenoid valve 10 through a pipeline. The gas analysis module includes an analysis chamber 5 , a vacuum gauge 6 and a gas analyzer 7 , and the analysis chamber 5 is respectively connected to the vacuum gauge 6 and the gas analyzer 7 through pipes. The calibration module includes a standard gas source 13 and a second regulating valve 14. The standard gas source 13 is connected to one end of the second regulating valve 14 through a pipeline, and the other end of the second regulating valve 14 is connected to the sampling sample connected to the valve group 3 and the flow restrictor 4 through a pipeline. tube.

Specifically, the process chamber 1 is a container whose gas composition is to be measured, such as an excimer laser discharge chamber, a synthesis tower in the urea industry, a vacuum chamber of an extreme ultraviolet (EUV) lithography machine, etc. It can also be other high pressure, normal pressure and vacuum container.

Specifically, one end of the sampling pipe 2 extends into the interior of the process chamber 1 for sampling at a designated position, and the other end is connected to the valve 3 so as to deliver the gas in the process chamber 1 to the device. In order to reduce the background of the device as much as possible, the material of the sampling tube 2 is preferably stainless steel or quartz glass, or silicon-based material or other materials. In addition, the gas flow state in the sampling tube 2 should be continuous flow, slip flow or molecular flow, and transition flow should be avoided as much as possible, so as to achieve non-destructive sampling. For high-pressure or atmospheric gases, continuous flow sampling is recommended; for vacuum environments, molecular flow sampling is recommended. Correspondingly, for continuous flow and molecular flow, it is recommended that the diameter d of the sampling tube 2 and the free path λ of gas molecules satisfy the relationship:

d≥10λ(1)

d≤λ/10(2)

Specifically, the valve group 3 is used to realize gas pressure reduction and on-off of the sampling pipeline. According to the different air pressures of the process chamber 1, a pressure reducing valve, a ball valve, a needle valve, a bellows stop valve and a combination thereof can be used.

Specifically, on the one hand, the restrictor 4 should realize the restriction of the flow of the gas, and reduce the intake flow and the evacuation pressure of the analysis chamber 5 . On the other hand, it is necessary to realize the molecular flow sampling of the gas in order to achieve non-destructive sampling. The restrictor 4 is preferably made of a capillary tube or a micropore, and a fine-tuning valve can also be used. The material of the restrictor 4 is preferably made of stainless steel or quartz glass, or silicon-based material or other materials.

Specifically, the analysis chamber 5 communicates with the restrictor 4 , and is also equipped with a vacuum gauge 6 , a gas analyzer 7 and a restrictor valve 8 . The analysis chamber 5 is generally made of stainless steel or aluminum alloy. The trace sampling gas of the restrictor 4 enters the analysis chamber 5 and is pumped away by the main pump 9 through the restrictor valve 8 , thereby forming a suitable vacuum degree in the analysis chamber 5 . The vacuum gauge 6 can measure the vacuum level of the analysis chamber 5 and provide data to the control system. The gas analysis module 7 measures and analyzes the gas components in the analysis chamber 5, and can use a quadrupole mass spectrometer, a time-of-flight mass spectrometer, an ion trap mass spectrometer or other gas analysis instruments. Generally speaking, the gas analyzer 7 needs to work in a suitable vacuum environment, so the working vacuum degree of the analysis chamber 5 is in the range of 10 ⁺² to 10 ^-5 Pa.

Specifically, one end of the restrictor valve 8 is connected to the analysis chamber 5 , and the other end is connected to the main pump 9 . The restrictor valve 8 is a vacuum valve with a through hole of a suitable size on the valve plate, which needs to be specially designed and manufactured. The main pump 9 is used to pump the ultimate vacuum or working vacuum to the analysis chamber 5, and can be an oil-free vacuum pump such as a molecular pump and an ion pump. When the valve plate of the restrictor valve 8 is opened, the main pump 9 is completely communicated with the analysis chamber 5, and the true pump 9 has the maximum pumping speed for the analysis chamber 5, and can pump the analysis chamber 5 with the ultimate vacuum. The ultimate vacuum degree is generally 10 ^-5 ~ 10 ^-9 Pa. When the valve plate of the restrictor valve 8 is closed, the main pump 9 communicates with the analysis chamber 5 through the opening on the valve plate of the restrictor valve 8 . Generally speaking, the size of the opening on the valve plate should take into account the needs of two aspects: ① The molecular flow pumping speed corresponding to the opening size can meet the needs of the analysis chamber 5 for working vacuum. ②The pumping speed of molecular flow corresponding to the opening size should not exceed 25% of the pumping speed of the main pump 9, so as to shield the fluctuation and selectivity of the pumping speed of the main pump 9, so as to achieve stable non-destructive sampling analysis.

Specifically, the fore pump 11 is connected to the main pump 9 through the solenoid valve 10 , and is used for pumping the fore vacuum to the main pump 9 . In addition, the backing pump 11 is connected to the gas pipeline between the valve group 3 and the restrictor 4 through the first regulating valve 12 . By adjusting the opening degree of the first regulating valve 12 , the required front-end air pressure or vacuum degree can be provided for the restrictor 4 . The backing pump 11 may be a Roots pump, a screw pump, a dry scroll pump, or the like.

Specifically, the standard gas source 13 is connected to the gas pipeline between the valve group 3 and the flow restrictor 4 through the second regulating valve 14 . The standard gas source 13 is used to provide high-purity standard gas for the gas analysis device, and the standard gas is a mixture of various gases with certain concentrations, such as Kr:Ar:Ne:He=20:10:2:1. By adjusting the opening of the second regulating valve 14, an appropriate amount of standard gas can be introduced.

Specifically, heaters are provided on the sampling pipe and the analysis chamber 5 of the gas sampling and analysis device. The heater can bake and degas the sampling pipeline and the analysis chamber 5 to obtain a good system background and improve the accuracy of gas analysis. In addition, the heater to bake and degas the analysis chamber 5 can also eliminate or reduce the contamination of the analysis chamber by hydrocarbons and the like.

Specifically, the gas sampling analysis device needs to be calibrated regularly to ensure the accuracy and repeatability of the analysis results. On the gas sampling and analysis device of FIG. 1 , the standard gas source 13 is connected to the gas pipeline between the valve group 3 and the flow restrictor 4 through the second regulating valve 14 . When the gas sampling and analysis device is calibrated, steps similar to the gas testing process are used to introduce the standard gas into the analysis chamber 5 through the second regulating valve 14 and the flow restrictor 4, and use the gas analyzer 7 to analyze the standard gas. If the analyzed gas composition and concentration are consistent with the standard gas, it means that the gas sampling and analysis device has been calibrated and can perform gas analysis. If the analyzed gas composition and concentration are inconsistent with the standard gas, the gas sampling and analysis device needs to be debugged until the calibration requirements are met. The debugging process of the gas sampling and analysis device can be baking heating, background extraction of the system, or adjustment of the parameters of the gas analyzer 7, etc.

Specifically, in FIG. 1 of the gas sampling and analysis device, the backing pump 11 is connected to the main pump 9 through the solenoid valve 10 on the one hand, and is used to pump the fore vacuum of the main pump 9; The gas pipeline connection between the valve block 3 and the restrictor 4 is used to provide the required front-end air pressure or vacuum for the restrictor 4 . When the process chamber 1 is at different air pressures or vacuum degrees, a single backing pump 11 may not be able to well meet the requirements of these two aspects. Therefore, a vacuum pump 15 can be added to meet the requirements of the above two aspects respectively. Another gas sampling and analysis device shown in FIG. 2 is different from the gas sampling and analysis device in FIG. 1 in that the sampling module is different. The gas sampling and analysis device in FIG. 2 The sampling module includes a process chamber, a valve group, a first regulating valve, a vacuum pump and a flow restrictor; the process chamber 1, the valve group 3 and the flow restrictor 4 are connected in sequence through a sampling pipe, one end of the sampling pipe is inserted into the process chamber 1, The other end is connected to one end of the valve group 3; the other end of the valve group 3 is connected to one end of the restrictor 4 through the sampling pipe; the other end of the restrictor 4 is connected to the gas analysis module through the sampling pipe; one end of the first regulating valve 12 is connected to the pipeline Connected to the valve group 3 and the sampling pipe connected to the flow restrictor 4 , the other end of the first regulating valve 12 is connected to the vacuum pump 16 through a pipeline.

Specifically, the fore pump 11 is connected to the main pump 9 through the solenoid valve 10, and is used to pump the fore vacuum of the main pump 9; The gas line connection is used to provide the required front air pressure or vacuum for the restrictor 4.

In the embodiment of the present application, by closing the valve group, the first regulating valve and the second regulating valve, and opening the vacuum gauge, the backing pump, the solenoid valve, the main pump and the restrictor valve, the analysis chamber is evacuated to the limit vacuum; when the analysis chamber is When the vacuum degree reaches the preset threshold, open the gas analysis module to monitor the analysis chamber in real time; when the gas analysis module does not detect polluting gas, close the gas analysis module and the restrictor valve, open the valve group and adjust the first adjustment Open the gas analysis module to analyze and test the sampled gas until the analysis chamber obtains the working vacuum; close the valve group and the first regulating valve, and open the restrictor valve to continue to pump the ultimate vacuum to the device; when the gas analysis module does not detect any polluting gas , close the gas sampling and analysis device and keep it in a vacuum state. The advantages of this application are: (1) online analysis of high pressure, normal pressure and vacuum gases, (2) increased gas sampling volume and improved system response speed, (3) elimination of molecular discrimination effect and pumping speed selection during gas sampling properties, so as to achieve non-destructive sampling analysis, (4) automatic calibration.

Referring to FIG. 3 , a schematic flowchart of a gas sampling and analysis method applied to a gas sampling and analysis device is provided for an embodiment of the present application. As shown in FIG. 3 , the method of the embodiment of the present application may include the following steps:

S101, close the valve group, the first regulating valve and the second regulating valve, and turn on the vacuum gauge, the backing pump, the solenoid valve, the main pumping valve and the limiting valve to pump the ultimate vacuum to the analysis chamber;

In a feasible implementation manner, by closing the valve group 3, the first regulating valve 12 and the second regulating valve 14, then opening the vacuum gauge 6, opening the foreline pump 11, the solenoid valve 10 and the restrictor valve 8 to the analysis chamber 5 Vacuum. When the analysis chamber 5 reaches a suitable vacuum degree (eg, less than 200 Pa), the main pump 9 is turned on. When the vacuum degree in the analysis chamber 5 meets the requirements, the gas analysis module 7 is turned on to monitor the system background in real time.

S102, when the vacuum degree of the analysis chamber reaches a preset threshold, turn on the gas analysis module to monitor the analysis chamber in real time;

In a feasible implementation manner, if the gas analyzer 7 detects that the system background is clean and there is no polluting gas, vacuum is continuously drawn until a good system background is obtained, and the background data is recorded. Otherwise, turn on the heater 15 to bake and degas the device to eliminate or reduce pollution until a good system background is obtained.

S103, when the gas analysis module does not detect polluting gas, close the gas analysis module and the restrictor valve, open the valve group and adjust the first regulating valve until the analysis chamber obtains a working vacuum, and then open the gas analysis module to analyze the sampled gas test;

In a feasible implementation, when a good system background is obtained, the gas analyzer 7 is closed, the restrictor valve 8 is closed, the valve group 3 is opened, and the first regulating valve 12 is adjusted until the analysis chamber 5 obtains a suitable vacuum degree. Turn on the gas analyzer 7, analyze and test the sampled gas, and record the data.

S104, closing the valve group and the first regulating valve, and opening the restrictor valve to continue pumping the ultimate vacuum to the device;

In a feasible implementation manner, after the gas analysis is completed, the valve group 3 and the first regulating valve 12 are closed, the restrictor valve 8 is opened, and the device is continuously evacuated. If the gas analyzer 7 detects that the system is free of contaminant gases, vacuum continues until a good system background is obtained. Otherwise, turn on the heater 15 to bake and degas the device to eliminate or reduce pollution until a good system background is obtained.

S105, when no polluting gas is detected by the gas analysis module, the gas sampling and analysis device is turned off to keep it in a vacuum state.

In a feasible implementation manner, after the sampling gas is exhausted, the gas sampling and analysis device is turned off to keep it in a vacuum state, so as to obtain a good system background in the next test. High-purity protective gas, such as 99.999% nitrogen, can also be filled in the gas sampling and analysis device.

For example, as shown in FIG. 4 , the typical operation flow of the gas sampling and analysis device includes first systematically extracting the background, then performing gas sampling and analysis, then performing sampling gas extraction, and finally closing the device.

Further, the gas sampling analysis device needs to be calibrated regularly to ensure the accuracy and repeatability of the analysis results. For example, when the gas sampling device shown in FIG. 1 is periodically calibrated, the standard gas source 13 is connected to the gas pipeline between the valve group 3 and the flow restrictor 4 through the second regulating valve 14 . Steps similar to the gas testing process are adopted. First, the standard gas is introduced into the analysis chamber 5 through the second regulating valve 14 and the flow restrictor 4, and the standard gas is analyzed by the gas analyzer 7. If the analyzed gas composition and concentration If it is consistent with the standard gas, it means that the gas sampling and analysis device is calibrated and can perform gas analysis. If the analyzed gas composition and concentration are inconsistent with the standard gas, the gas sampling and analysis device needs to be debugged until the calibration requirements are met. The debugging process of the gas sampling and analysis device can be baking heating, background extraction of the system, or adjustment of the parameters of the gas analyzer 7, etc.

In the embodiment of the present application, by closing the valve group, the first regulating valve and the second regulating valve, and opening the vacuum gauge, the backing pump, the solenoid valve, the main pump and the restrictor valve, the analysis chamber is evacuated to the limit vacuum; when the analysis chamber is When the vacuum degree reaches the preset threshold, open the gas analysis module to monitor the analysis chamber in real time; when the gas analysis module does not detect polluting gas, close the gas analysis module and the restrictor valve, open the valve group and adjust the first adjustment Open the gas analysis module to analyze and test the sampled gas until the analysis chamber obtains the working vacuum; close the valve group and the first regulating valve, and open the restrictor valve to continue to pump the ultimate vacuum to the device; when the gas analysis module does not detect any polluting gas , close the gas sampling and analysis device and keep it in a vacuum state. The advantages of this application are: (1) online analysis of high pressure, normal pressure and vacuum gases, (2) increased gas sampling volume and improved system response speed, (3) elimination of molecular discrimination effect and pumping speed selection during gas sampling properties, so as to achieve non-destructive sampling analysis, (4) automatic calibration.

Those of ordinary skill in the art can understand that all or part of the processes in the methods of the above embodiments can be implemented by instructing the relevant hardware through a computer program, and the program can be stored in a computer-readable storage medium, and the program is During execution, it may include the processes of the embodiments of the above-mentioned methods. Wherein, the storage medium can be a magnetic disk, an optical disk, a read-only storage memory, or a random storage memory, and the like.

The above disclosures are only the preferred embodiments of the present application, and of course, the scope of the rights of the present application cannot be limited by this. Therefore, equivalent changes made according to the claims of the present application are still within the scope of the present application.

Claims (10)

1. A gas sampling analysis apparatus, the apparatus comprising:

the device comprises a vacuum acquisition module, a sampling module and a gas analysis module; wherein,

the gas analysis module is respectively connected with the vacuum acquisition module and the sampling module; wherein,

the vacuum acquisition module comprises a flow limiting valve, and when the flow limiting valve is opened and closed, the ultimate vacuum and the working vacuum of the gas analysis module are respectively realized; wherein,

the flow limiting valve is a vacuum valve with a through hole with a proper size formed in a valve plate.

2. A gas sampling analysis apparatus according to claim 1, the apparatus further comprising:

a calibration module; wherein the calibration module is connected with the sampling module.

3. A gas sampling analysis apparatus according to claim 1 or 2,

the vacuum acquisition module comprises a flow limiting valve, a main pump, an electromagnetic valve and a backing pump; the flow limiting valve, the main pumping pump, the electromagnetic valve and the backing pump are sequentially connected through pipelines; one end of the flow limiting valve is connected to the main pump through the pipeline, and the other end of the flow limiting valve is connected to the gas analysis module through the pipeline; wherein, the demand of the trompil size on the restriction valve plate includes at least: firstly, the molecular flow pumping speed corresponding to the size of the opening meets the requirement of the vacuum pumping of the analysis chamber. And the pumping speed of the molecular flow corresponding to the size of the opening is not more than 25 percent of the pumping speed of the main pump.

4. A gas sampling analysis apparatus according to claim 3,

the sampling module comprises a process chamber, a valve group, a first regulating valve and a current limiter; the process chamber, the valve group and the flow restrictor are sequentially connected through a sampling pipe, one end of the sampling pipe is inserted into the process chamber, and the other end of the sampling pipe is connected with one end of the valve group; the other end of the valve group is connected to one end of the flow restrictor through the sampling pipe; the other end of the flow restrictor is connected to the gas analysis module through the sampling pipe; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the flow restrictor through a pipeline, and the other end of the first regulating valve is connected to the vacuum acquisition module through a pipeline.

5. A gas sampling analysis apparatus according to claim 4,

the gas analysis module comprises an analysis chamber, a vacuum gauge and a gas analyzer, wherein the analysis chamber is respectively connected with the vacuum gauge and the gas analyzer through pipelines; wherein,

the analysis chamber can also be respectively connected with the vacuum gauge and the gas analyzer through valves;

wherein, the gas analysis module can at least select a quadrupole mass spectrometer, a time-of-flight mass spectrometer and an ion trap mass spectrometer; wherein;

heaters are arranged on the pipeline and the analysis chamber, and the heaters can bake and degas the sampling pipeline and the analysis chamber.

6. A gas sampling analysis apparatus according to claim 4,

the calibration module comprises a standard gas source and a second regulating valve, the standard gas source is connected with one end of the second regulating valve through a pipeline, and the other end of the second regulating valve is connected to the valve bank and the sampling pipe connected with the flow restrictor through a pipeline; wherein, the standard gas source can provide high-purity standard gas for the gas analysis device, and the standard gas is a mixture of a plurality of gases with determined concentration.

7. A gas sampling analysis apparatus according to claim 4,

the sampling module comprises a process chamber, a valve group, a first regulating valve, a vacuum pump and a current limiter; the process chamber, the valve group and the flow restrictor are sequentially connected through a sampling pipe, one end of the sampling pipe is inserted into the process chamber, and the other end of the sampling pipe is connected with one end of the valve group; the other end of the valve group is connected to one end of the flow restrictor through the sampling pipe; the other end of the flow restrictor is connected to the gas analysis module through the sampling pipe; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the flow restrictor through a pipeline, and the other end of the first regulating valve is connected to a vacuum pump through a pipeline. Wherein, the flow restrictor at least adopts a capillary tube, a micropore and a trim valve, and preferentially adopts the capillary tube or the micropore.

8. A gas sampling analysis device according to any one of claims 4 to 7,

when the process cavity is filled with high-pressure or normal-pressure gas, continuous flow sampling is adopted; and when the process cavity is in a vacuum environment, molecular flow sampling is adopted. Accordingly, the diameters of the sampling pipes and the free paths of the gas molecules passing through the sampling pipes are respectively as follows:

d≥10λ (1)

d≤λ/10 (2)

wherein d is the diameter of the sampling tube, and lambda is the free path of gas molecules.

9. A gas sampling analysis apparatus according to claim 5, wherein the vacuum acquisition module is configured to evacuate the analysis chamber; the sampling module is used for acquiring the gas to be detected in the analysis chamber; the gas analysis module is used for detecting and analyzing the gas to be detected in the analysis chamber; the calibration module is used for periodically calibrating the gas sampling and analyzing device.

10. A method of gas sampling analysis using the apparatus of any one of claims 1 to 9, the method comprising:

closing the valve group, the first regulating valve and the second regulating valve, and opening the vacuum gauge, the backing pump, the electromagnetic valve, the main pump and the flow limiting valve to carry out ultimate vacuum pumping on the analysis chamber;

when the vacuum degree of the analysis chamber reaches a preset threshold value, starting a gas analysis module to monitor the analysis chamber in real time;

when the gas analysis module does not monitor the polluting gas, the gas analysis module and the flow limiting valve are closed, the valve bank is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to carry out analysis test on the sampled gas;

closing the valve group and the first regulating valve, and opening the flow limiting valve to continue to carry out ultimate vacuum pumping on the device;

and when the gas analysis module does not monitor the polluting gas, closing the gas sampling analysis device to keep the gas sampling analysis device in a vacuum state.

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