CN113092412B - Online detection device and method for multi-component trace gas under negative pressure state - Google Patents
Online detection device and method for multi-component trace gas under negative pressure state Download PDFInfo
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Abstract
The invention provides a device and a method for detecting multi-component trace gas on line under a negative pressure state, wherein the gas to be detected is introduced into a ring-down cavity, and a laser control center controls waves emitted by a tunable laserLambda of length 1 、λ 2 、λ 3 The optical switch controls the wavelength lambda 1 、λ 2 、λ 3 The laser signal of one of the laser signals is divided into two laser signals with the energy ratio of 99:1 through an optical beam splitter, the laser signal with 99% energy is coupled into an optical ring-down cavity through an optical isolator, the laser signal with 1% energy is transmitted into a calibration system and corresponds to one of the laser signals according to the wavelength, a photoelectric converter captures calibration information and transmits the calibration information to a central data processing and control center, a photoelectric detector captures the laser signal transmitted from the optical ring-down cavity and transmits the captured information to the central data processing and control center, ring-down time is obtained, and the concentration of the gas to be detected is calculated according to the ring-down time.
Description
Technical Field
The invention relates to the technical field of gas detection, in particular to a device and a method for detecting multi-component trace gas on line under a negative pressure state.
Background
In the production process of high-purity gas (background gas), the high-purity gas (background gas) contains a plurality of different kinds of impurity gas molecules, and the existence of the impurities can influence the quality of the high-purity gas (background gas).
The existing gas detection methods (mass spectrometry, chromatography, spectrometry, capacitance method, electrochemical method and the like) have the problems of low sensitivity, low response speed, poor stability, incapability of on-line multi-component detection and the like, and can not meet the requirement of the production process of high-purity gas (background gas). In order to ensure or improve the quality of high-purity gas (background gas), it is important to provide an online detection method for multi-component trace gas to solve the problem.
Molecular absorption lines are highly specific and can be used to identify the molecular content of any medium (e.g., gas) that is capable of passing light. The molecular absorption spectrum method can solve the problems of low sensitivity, slow response speed and poor stability of the existing gas detection methods. The characteristic absorption peaks corresponding to the impurity gas molecules of different types are respectively selected, so that the problem of multi-component gas detection can be solved.
Although molecular absorption lines are highly specific, the background gas and part of the characteristic absorption lines of different impurity molecules sometimes cross or overlap, which in this case affects the accuracy of the measurement.
The molecular characteristic absorption spectrum is mainly affected by the temperature and pressure of the test environment. In order to solve the problem that the intersection or overlapping of absorption lines affects the test accuracy, the multi-component trace gas online detection method provided by the patent is implemented in a negative pressure state.
Disclosure of Invention
The invention aims to provide a multi-component trace gas detection device and method under a negative pressure state, and the device and method have the advantages of high sensitivity, high response speed, high accuracy, high stability and the like compared with the existing detection method.
In order to solve the above technical problems, the present invention provides a multi-component trace gas detection device under negative pressure, which includes:
the device comprises a laser control center, a plurality of tunable lasers, a polarization maintaining optical fiber, an optical switch, an optical beam splitter, an optical isolator, an optical fiber collimator, an air tank, a pressure control center, a plurality of high-reflection mirrors, a reaction tower, a vacuum pump, a plurality of ring-down cavities, a photoelectric detector, a central data processing and control center, a plurality of optical switches, a laser calibration center and a photoelectric converter.
The laser control center is electrically connected with the tunable lasers; the photoelectric detector is electrically connected with the central data processing and control center; the laser control center is electrically connected with the central data processing and control center; the optical switches are electrically connected with the central data processing and control center; the high-reflection mirrors are mechanically fixed in the ring-down cavity; the polarization maintaining optical fiber, the optical beam splitter, the optical isolator and the optical fiber collimator are mechanically connected; the pressure control center is electrically connected with the central data processing and control center; the photoelectric detector and the photoelectric converter are electrically connected with the central data processing and control center; the pressure control center and the vacuum pump are mechanically connected with the ring-down cavity.
The optical fiber collimator consists of an optical fiber and a collimating lens, wherein the collimating lens can be a C-lens, a self-focusing lens or a ball lens system; the ball lens system mainly comprises a prism, a positive lens and a negative lens.
The invention also provides a multi-component trace gas measurement method by adopting the measurement device, which comprises the following steps:
firstly, introducing a gas to be detected containing various impurities into the ring-down cavity;
secondly, controlling the inside of the ring-down cavity to be in a negative pressure state through the pressure control center and the vacuum pump, and setting different pressures according to use requirements;
thirdly, the laser control center controls the tunable laser to emit laser signals with different wavelengths;
step four, the central data processing and control center enables laser signals with different wavelengths to selectively pass through one or more through the regulation and control optical switch, and the laser signals are divided into two laser signals with the energy ratio of 99:1 through the beam splitter;
fifthly, transmitting the 99% energy laser signal to an optical isolator through a polarization maintaining optical fiber transmission optical switch, and transmitting the 99% energy laser signal to the optical switch after being collimated by an optical fiber collimator after passing through the optical isolator;
step six, the central data processing and control center enables the laser signals with different wavelengths to pass through the light collimator through the regulation and control optical switch, and then the laser signals are coupled into the ring-down cavity and resonate with an optical system consisting of a high reflection mirror positioned in the ring-down cavity; the resonant optical signal is transmitted between the two high-reflection mirrors in a reflection mode in the optical ring-down cavity;
seventhly, transmitting laser signals with 1% of energy to an optical switch through a polarization maintaining optical fiber, enabling laser signals with different wavelengths to be correspondingly coupled to a characteristic absorption spectrum calibration system of gas to be tested by a central data processing and control center through regulating the optical switch, capturing calibration information in the characteristic absorption spectrum calibration system of the gas to be tested by a photoelectric converter in real time and transmitting the calibration information to the central data processing and control center, and controlling the laser control center to adjust the wavelength of the emitted laser signals according to the obtained calibration information by the central data processing and control center to perform self calibration;
eighth, the electric detector captures the laser signal transmitted from the ring-down cavity in real time, monitors the energy change condition of the laser signal in the ring-down cavity in real time, and transmits the monitored information to the central data processing and control center after photoelectric conversion to obtain the ring-down time tau of the laser signal;
ninth, after the ring-down time is measured, the concentration of the impurity gas in the gas to be measured can be calculated according to the lambert beer law,
wherein N is m The impurity gas concentration is given, and m is the impurity gas type; τ is the ring down time measured when the gas to be measured is absorbed, τ 0 For the ring down time measured without absorption of the gas to be measured, c is the speed of light, σ (λ) m ) The absorption cross sections correspond to characteristic absorption peaks of the impurity gas respectively.
Sometimes, the gas to be tested can be toxic gas, so that the tail gas treatment is required to be carried out in real time in the testing process, and the tested tail gas is collected into the reaction tower.
The beneficial effects of the invention are that
The multi-component trace gas detection method under the negative pressure state is based on the negative pressure state, and the contents of m (m is more than or equal to 3) kinds of impurity gases in the gas to be detected are measured by utilizing lasers with various wavelengths (the wavelength types of the lasers and the number of the ring-down cavities are more than or equal to 3), so that the on-line monitoring of the multi-component impurity gases can be realized. The method can self-calibrate due to the introduction of the laser calibration center, and has the advantages of high accuracy, small error, high sensitivity, high response speed, high stability and the like, and has high practicability.
Drawings
FIG. 1 is a schematic diagram of a detection device;
1. a laser control center; 2. a first tunable laser; 3. polarization maintaining optical fiber; 4. a first optical switch; 5. a beam splitter; 6. an optical isolator; 7. an optical fiber collimator; 8. an air tank; 9. a pressure control center; 10. a high reflection mirror A; 11. a reaction tower; 12. a vacuum pump; 13. a ring-down cavity A; 14. a ring-down cavity B; 15. a ring-down cavity C; 16. a high reflection mirror B; 17. a photodetector; 18. a central data processing and control center; 19. a third optical switch; 19. a laser calibration center; 21. a photoelectric converter; 22. a third tunable laser; 23. a second tunable laser; 24. and a second optical switch.
Detailed Description
The invention provides a multi-component trace gas detection device under a negative pressure state, which comprises:
the device comprises a laser control center, a plurality of tunable lasers, a polarization maintaining optical fiber, an optical switch, an optical beam splitter, an optical isolator, an optical fiber collimator, an air tank, a pressure control center, a plurality of high-reflection mirrors, a reaction tower, a vacuum pump, a plurality of ring-down cavities, a photoelectric detector, a central data processing and control center, a plurality of optical switches, a laser calibration center and a photoelectric converter.
The laser control center is electrically connected with the tunable lasers; the photoelectric detector is electrically connected with the central data processing and control center; the laser control center is electrically connected with the central data processing and control center; the optical switches are electrically connected with the central data processing and control center; the high-reflection mirrors are mechanically fixed in the ring-down cavity; the polarization maintaining optical fiber, the optical beam splitter, the optical isolator and the optical fiber collimator are mechanically connected; the pressure control center is electrically connected with the central data processing and control center; the photoelectric detector and the photoelectric converter are electrically connected with the central data processing and control center; the pressure control center and the vacuum pump are mechanically connected with the ring-down cavity.
The optical fiber collimator consists of an optical fiber and a collimating lens, wherein the collimating lens can be a C-lens, a self-focusing lens or a ball lens system; the ball lens system mainly comprises a prism, a positive lens and a negative lens.
The invention also provides a multi-component trace gas measurement method by adopting the measurement device, which comprises the following steps:
firstly, introducing a gas to be detected containing m impurity gases into an optical ring-down cavity, wherein m is more than or equal to 3, and m=3 is selected most preferably;
secondly, controlling the inside of the ring-down cavity to be in a negative pressure state through the pressure control center and the vacuum pump, and setting different pressures according to use requirements;
thirdly, the laser control center controls the three tunable lasers to emit m laser signals with different wavelengths;
step four, the central data processing and control center enables the m laser signals with different wavelengths to selectively pass through one or more through the regulation and control optical switch, and the m laser signals are divided into two laser signals with the energy ratio of 99:1 through the beam splitter;
fifthly, transmitting the 99% energy laser signal to an optical isolator through a polarization maintaining optical fiber transmission optical switch, and transmitting the 99% energy laser signal to the optical switch after being collimated by an optical fiber collimator after passing through the optical isolator;
step six, the central data processing and control center enables the laser signals with three different wavelengths to pass through the light collimator through the regulation and control optical switch, and then to be coupled into the ring-down cavity and resonate with an optical system consisting of a high-reflection mirror positioned in the ring-down cavity; the resonant optical signal is transmitted between the two high-reflection mirrors in a reflection mode in the optical ring-down cavity;
seventhly, transmitting laser signals with 1% of energy to an optical switch through a polarization maintaining optical fiber, enabling laser signals with different wavelengths to be correspondingly coupled to a characteristic absorption spectrum calibration system of gas to be tested by a central data processing and control center through regulating the optical switch, capturing calibration information in the characteristic absorption spectrum calibration system of the gas to be tested by a photoelectric converter in real time and transmitting the calibration information to the central data processing and control center, and controlling the laser control center to adjust the wavelength of the emitted laser signals according to the obtained calibration information by the central data processing and control center to perform self calibration;
eighth, the electric detector captures the laser signal transmitted from the ring-down cavity in real time, monitors the energy change condition of the laser signal in the ring-down cavity in real time, and transmits the monitored information to the central data processing and control center after photoelectric conversion to obtain the ring-down time tau of the laser signal;
ninth, after the ring-down time is measured, the concentration of the impurity gas in the gas to be measured can be calculated according to the lambert beer law,
wherein N is m The impurity gas concentration is given, and m is the impurity gas type; τ is the ring down time measured when the gas to be measured is absorbed, τ 0 For the ring down time measured without absorption of the gas to be measured, c is the speed of light, σ (λ) m ) The absorption cross sections correspond to characteristic absorption peaks of the impurity gas respectively.
The following examples and drawings are used to describe embodiments of the present invention in detail, thereby solving the technical problems by applying the technical means to the present invention, and realizing the technical effects can be fully understood and implemented accordingly.
Fig. 1 shows a multi-component trace gas online detection device under a negative pressure state, which adopts the following method to carry out multi-component trace gas online detection.
Firstly, introducing gas to be detected in an air storage tank 8 into the ring-down chambers 13, 14 and 15, and then setting the interiors of the ring-down chambers 13, 14 and 15 into a negative pressure state (50 torr, 80torr, 90torr and the like according to test requirements) through a vacuum pump 20 and a pressure control center 17; the tail gas flowing through the vacuum pump 12 is introduced into the reaction tower 11 for tail gas treatment or recycling.
The laser control center 1 controls the wavelength lambda of laser signals emitted by the three tunable lasers 2, 22, 23 1 、λ 2 、λ 3 Wavelength lambda 1 、λ 2 、λ 3 The wavelength corresponding to the characteristic absorption peak of the impurity gas to be detected;
the laser signal is divided into energy ratio 99 by the optical beam splitter 5 after passing through the polarization maintaining optical fiber 3 and the first optical switch 4: 1, (wherein a polarization maintaining optical fiber 3 is arranged to ensure that the polarization direction of the laser signal is unchanged, improve the coherent signal to noise ratio so as to improve the precision, and a first optical switch 4 is used for carrying out line switching on an optical transmission line), 99% of the energyThe laser signal is transmitted to the optical isolator 6 through the polarization maintaining fiber 3, and the central data processing and control center 18 regulates the second optical switch 24 to make the wavelength lambda 1 、λ 2 、λ 3 After passing through the optical collimator, the laser signals are coupled into the ring-down cavity and resonated with the ring-down cavity, (wherein the optical isolator 6 is used for ensuring unidirectional transmission of the laser signals, the optical collimator 7 is used for enabling the light passing through each point of the optical isolator 6 to be changed into a parallel collimated light beam to enter the ring-down cavity 21), the laser signals with 1% energy are transmitted to the third optical switch 19 through the polarization maintaining fiber 3, and the central data processing and control center 18 controls the third optical switch 19 to transmit the wavelength lambda 1 、λ 2 、λ 3 The calibrated information is transmitted to a central data processing and control center 18 after being converted by a photoelectric converter 21, the laser signals are divided into two beams by utilizing an optical beam splitter 5, one beam is tested, the other beam is calibrated, self calibration is realized, the wavelength of the incident laser signals is ensured to be stable, a photoelectric detector 17 captures the laser signals transmitted from the ring-down cavities 13, 14 and 15 in real time, the energy of the laser signals is monitored in real time to change in the ring-down cavities 13, 14 and 15, the monitored information is transmitted to the central data processing and control center 18 after being subjected to photoelectric conversion, the ring-down time tau of the laser signals is obtained, and the concentration of the gas to be measured can be calculated according to the lambert law after the ring-down time is measured,
wherein N is 1 、N 2 、N 3 For the concentration of the impurity gas to be measured, τ is the ring-down time measured when the impurity gas to be measured is absorbed, τ 0 For the ring-down time measured without the absorption of the impurity gas to be measured, c is the speed of light, σ (λ) 1 )、σ(λ 2 )、σ(λ 3 ) Respectively corresponding absorption cross sections of characteristic absorption peaks of different impurity gases to be detected, and calculating N 1 、N 2 、N 3 The concentration value is different to be measured of impurity gasConcentration.
The transmission direction of the 99% energy laser signal is preferably controlled by the fiber collimator 7 before the 99% energy laser signal is incident on the ring down cavity, while the two high reflection mirrors 10, 16 in the ring down cavities 13, 14, 15 are adjusted so that the 99% energy laser signal is coaxial with the optical system in the ring down cavities 13, 14, 15.
All of the above-described primary implementations of this intellectual property are not intended to limit other forms of implementing this new product or new method. Those skilled in the art will utilize this important information and the above modifications to achieve a similar implementation. However, all modifications or adaptations belong to the reserved rights based on the new products of the invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (5)
1. The multi-component trace gas measurement method adopts a multi-component trace gas detection device under a negative pressure state to carry out measurement, and the device comprises a laser control center, a plurality of tunable lasers, a polarization maintaining optical fiber, an optical switch, an optical beam splitter, an optical isolator, an optical fiber collimator, an air storage tank, a pressure control center, a plurality of high-reflection mirrors, a reaction tower, a vacuum pump, a plurality of ring-down cavities, a photoelectric detector, a central data processing and control center, a plurality of optical switches, a laser calibration center and a photoelectric converter, and is characterized by comprising the following steps:
firstly, introducing a gas to be detected containing various impurities into the ring-down cavity;
secondly, controlling the inside of the ring-down cavity to be in a negative pressure state through the pressure control center and the vacuum pump, and setting different pressures according to use requirements;
thirdly, the laser control center controls the tunable laser to emit laser signals with different wavelengths;
step four, the central data processing and control center enables laser signals with different wavelengths to selectively pass through one or more through the regulation and control optical switch, and the laser signals are divided into two laser signals with the energy ratio of 99:1 through the beam splitter;
fifthly, transmitting the 99% energy laser signal to an optical isolator through a polarization maintaining optical fiber transmission optical switch, and transmitting the 99% energy laser signal to the optical switch after being collimated by an optical fiber collimator after passing through the optical isolator;
step six, the central data processing and control center enables the laser signals with different wavelengths to pass through the light collimator through the regulation and control optical switch, and then the laser signals are coupled into the ring-down cavity and resonate with an optical system consisting of a high reflection mirror positioned in the ring-down cavity; the resonant optical signal is transmitted between the two high-reflection mirrors in a reflection mode in the optical ring-down cavity;
seventhly, transmitting laser signals with 1% of energy to an optical switch through a polarization maintaining optical fiber, enabling laser signals with different wavelengths to be correspondingly coupled to a characteristic absorption spectrum calibration system of gas to be tested by a central data processing and control center through regulating the optical switch, capturing calibration information in the characteristic absorption spectrum calibration system of the gas to be tested by a photoelectric converter in real time and transmitting the calibration information to the central data processing and control center, and controlling the laser control center to adjust the wavelength of the emitted laser signals according to the obtained calibration information by the central data processing and control center to perform self calibration;
eighth, the electric detector captures the laser signal transmitted from the ring-down cavity in real time, monitors the energy change condition of the laser signal in the ring-down cavity in real time, and transmits the monitored information to the central data processing and control center after photoelectric conversion to obtain the ring-down time tau of the laser signal;
ninth, after the ring-down time is measured, the concentration of the impurity gas in the gas to be measured can be calculated according to the lambert beer law,
wherein, the liquid crystal display device comprises a liquid crystal display device,N m for the concentration of the impurity gas,mis an impurity gas species;τto have a measured ring down time when the gas to be measured is absorbed,τ 0 for the ring down time measured without the absorption of the gas to be measured,cin order to achieve the light velocity, the light beam is,σ(λ m ) The absorption cross sections correspond to characteristic absorption peaks of the impurity gas respectively.
2. The multi-component trace gas measurement method according to claim 1, wherein: the laser control center is electrically connected with the tunable lasers; the photoelectric detector is electrically connected with the central data processing and control center; the laser control center is electrically connected with the central data processing and control center; the optical switches are electrically connected with the central data processing and control center; the high-reflection mirrors are mechanically fixed in the ring-down cavity; the polarization maintaining optical fiber, the optical beam splitter, the optical isolator and the optical fiber collimator are mechanically connected; the pressure control center is electrically connected with the central data processing and control center; the photoelectric detector and the photoelectric converter are electrically connected with the central data processing and control center; the pressure control center and the vacuum pump are mechanically connected with the ring-down cavity.
3. The multi-component trace gas measurement method according to claim 1, wherein: the optical fiber collimator consists of an optical fiber and a collimating lens.
4. A multi-component trace gas measurement method according to claim 3, wherein: the collimating lens may be a C-lens, a self-focusing lens, or a ball lens system.
5. The multi-component trace gas measurement method according to claim 4, wherein: the ball lens system mainly comprises a prism, a positive lens and a negative lens.
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