CN111413321A - Optical fiber Raman spectrum gas analysis device - Google Patents
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- CN111413321A CN111413321A CN202010367086.7A CN202010367086A CN111413321A CN 111413321 A CN111413321 A CN 111413321A CN 202010367086 A CN202010367086 A CN 202010367086A CN 111413321 A CN111413321 A CN 111413321A
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Abstract
The invention discloses a fiber Raman spectrum gas analysis device, belonging to the technical field of gas analysis, comprising: the device comprises a laser, a light beam coupling device, a gas sample chamber, a collimation and beam splitting device and a photoelectric imaging receiving device; the light beam coupling device couples the laser into the gas sample chamber; the laser and the gas to be detected in the hollow optical fiber core act to generate Raman scattering; the collimation beam splitting device collimates the mixed light beam and then separates out laser, and the light beam only containing scattering signals is transmitted to the photoelectric imaging receiving device; and the photoelectric imaging receiving device performs digital spatial filtering on the forward scattering signal to obtain the Raman spectrum of the gas to be measured. The invention generates enhanced Raman scattering signals by the action of the gas to be detected and laser in the hollow optical fiber, collects forward signals by using the photoelectric imaging receiving device, and implements digital spatial filtering, thereby reducing background signals of the gas sample chamber, solving the problem of difficult detection of trace components in Raman gas analysis and improving the detection sensitivity of the system.
Description
Technical Field
The invention belongs to the technical field of gas analysis and detection, and particularly relates to a fiber Raman spectrum gas analysis device.
Background
The phenomenon in which the excitation light is scattered by molecules and the frequency of the scattered light is changed is called raman scattering. When the intensity of the excitation light is weak, the intensity of the scattered light is proportional to the intensity of the excitation light and the number of scattered molecules, and the raman scattering is often called linear raman scattering or spontaneous raman scattering, and the linear correlation between the signal intensity and the number of scattered molecules makes the raman scattering widely used for chemical analysis. Because the Raman cross section and the molecular number density of the gas are relatively small, the Raman scattering intensity is very weak, the gas detection based on the Raman spectrum is limited, and the improvement of the intensity of a gas signal is particularly important. In recent years, the research and development of gas raman detection are dedicated to improve the detection sensitivity of the device and increase the application range thereof, wherein the main means of the research and development include enhancing raman signals and reducing signal background. For gas detection, the main technical methods for enhancing signals currently include various forms such as hollow fiber enhancement, resonant cavity enhancement and multi-optical path enhancement. The hollow optical fiber serves as a sample gas chamber, can remarkably increase Raman scattering signals, and has high application value.
In the optical fiber enhanced Raman spectrum technology, the selection of the optical fiber has great influence on the signal background and the signal to noise ratio, most of the published results at present adopt band gap type hollow photonic crystal fibers or capillary tubes internally plated with metal, but the former has the disadvantages of low gas circulation speed due to small core diameter and easy gas retention of small and dense cladding holes, and is not beneficial to the quick gas update; the latter has high transmission loss, and the excitation light leaking into the glass cladding also brings fluorescence and silica raman background. It is a major task to find more suitable hollow-core optical fibers.
A human body respirometer detection method (patent No. CN107421942A) based on hollow-core photon crystal optical fiber and Raman spectrum combines optical fiber reinforcement and cavity reinforcement technology, optical fiber Bragg gratings are arranged at two ends of the hollow-core optical fiber to form a resonant cavity, incident light oscillates back and forth in the optical fiber, the number of molecules participating in Raman scattering action is increased, and therefore the strength of gas signals is improved, but imperfect coupling can also cause the increase of fluorescence and silicon dioxide Raman backgrounds. The preparation method of the hollow-core optical fiber SERS probe and the harmful gas detection system (patent number CN109239050A) combine optical fiber enhancement and surface-enhanced Raman spectroscopy technology, gold and silver nanoparticles are assembled on the inner surface of a fiber core of a hollow-core optical fiber, or prepared metal nanoparticles are uniformly mixed with a sample to be detected and then subjected to Raman detection to form a suspended metal nanoparticle substrate, signals can be greatly improved, but the preparation cost of the nanoparticles is high, and any pollution on the surfaces of the nanoparticles (such as adsorption generated by last gas measurement) can influence the accuracy of measurement and is not suitable for repeated online detection.
Disclosure of Invention
In view of the above defects or improvement requirements of the prior art, the present invention provides a fiber raman spectroscopy gas analysis apparatus, thereby solving the technical problems of high signal background and low analysis sensitivity of a gas analysis system.
To achieve the above object, according to one aspect of the present invention, there is provided a fiber raman spectroscopy gas analysis apparatus comprising: the device comprises a laser, a light beam coupling device, a gas sample chamber, a collimation and beam splitting device and a photoelectric imaging receiving device;
the light beam coupling device is used for coupling laser emitted by the laser into the gas sample chamber;
the gas sample chamber is used for enabling the coupled laser to act with gas molecules to be detected in a hollow optical fiber core of the gas sample chamber to generate Raman scattering, and transmitting a mixed beam of a forward scattering signal and the laser to the collimation beam splitting device;
the collimation beam splitting device is used for collimating the mixed light beam, separating laser in the mixed light beam, and transmitting the light beam only containing the forward scattering signal to the photoelectric imaging receiving device;
and the photoelectric imaging receiving device is used for collecting the forward scattering signals and carrying out digital spatial filtering on the forward scattering signals to obtain the Raman spectrum of the gas to be detected.
Preferably, the light beam coupling device comprises a laser line filter and a focusing coupling lens; the laser line filter is used for filtering fluorescent components in laser generated by the laser; the focusing coupling lens is used for converging the laser and coupling the laser into the hollow-core optical fiber.
Preferably, the gas sample chamber comprises a gas bomb, a pipeline, a hollow-core optical fiber, a fixing device and a vacuum pump;
the gas storage bottle is used for storing the gas to be detected; the hollow optical fiber is used for enabling the gas to be detected to act with laser to generate Raman scattering; the fixing device is used for fixing two ends of the hollow optical fiber; the vacuum pump is used for evacuating the gas in the hollow-core optical fiber when the gas to be detected is updated; the gas storage bottle is connected with the hollow optical fiber through the pipeline, the hollow optical fiber is connected with the vacuum pump through the pipeline, and the pipeline is used for conveying the gas to be detected.
Preferably, the gas sample chamber further comprises a solenoid valve; the electromagnetic valve is arranged between the gas storage bottle and the hollow optical fiber and used for controlling the on-off of the gas path.
Preferably, the gas sample chamber further comprises a gas pressure gauge; the barometer is arranged between the electromagnetic valve and the hollow-core optical fiber and used for displaying the air pressure of the gas to be detected in the pipeline.
Preferably, the hollow-core optical fiber is a hypocycloid-type Kagomse hollow-core optical fiber.
Preferably, the collimating and beam-splitting device comprises a collimating lens, a dichroic mirror, a light beam blocking device and a long-pass filter;
the collimating lens is used for converting the mixed light beam output by the gas sample chamber into a collimated parallel light beam; the dichroic mirror is used for separating laser light in the mixed light beam from a forward scattering signal; the beam blocking device is used for absorbing laser in the mixed beam reflected by the dichroic mirror; the long-pass filter is used for filtering residual laser in the forward scattering signals.
Preferably, the photoelectric imaging receiving device comprises an optical radiation collecting lens, a spectrometer, a detector and a data processing device;
the spectrometer is used for obtaining the spectral distribution of the forward scattering signals which are collected by the optical radiation collecting lens and penetrate through the long-pass filter; the detector is used for imaging the spectral distribution of the forward scattering signal; and the data output end of the detector is connected with the data processing device, and the data processing device is used for controlling the acquisition and processing of the forward scattering signal, implementing digital spatial filtering and obtaining the Raman spectrum of the gas to be detected.
Preferably, the data processing means is further adapted to adjust the focus of the optical radiation collection lens to focus the forward scatter signal onto the detector.
Preferably, the detector is a CCD array detector.
Generally, compared with the prior art, the above technical solution conceived by the present invention has the following beneficial effects:
1. the invention combines the forward Raman scattering signal collection with the digital spatial filtering of an imaging spectrometer, obtains a spectrum with low background, effectively reduces the signal background and noise, improves the sensitivity of analysis, is simultaneously suitable for the detection of trace component gas, and has wide application prospect in the aspects of environmental gas sensing, respiratory gas analysis, industrial monitoring and the like;
2. the invention collects forward Raman scattering signals, avoids Raman fluorescence background generated during laser coupling, reduces noise and improves signal-to-noise ratio;
3. the invention uses the hypocycloid Kagomse hollow fiber to reduce the transmission loss, and the fiber core mode and the cladding mode have only a small amount of spatial overlap;
4. the invention adopts the imaging spectrometer to implement digital spatial filtering, further simplifies the experimental device,
the difficulty of light path adjustment is reduced.
Drawings
FIG. 1 is a schematic block diagram of one embodiment of the present invention;
FIG. 2 is a schematic diagram of the structure of a gas sample chamber of one embodiment of the present invention.
The same reference numbers will be used throughout the drawings to refer to the same or like elements or structures, wherein: a laser 1; a laser line filter 2; a focusing coupling lens 3; a gas sample cell 4; a collimating lens 5; a dichroic mirror 6; a beam blocking device 7; a long pass filter 8; an optical radiation collecting lens 9; a spectrometer 10; a detector 11; a data processing device 12; a gas cylinder 13; a pipe 14; a solenoid valve 15; a barometer 16; a fixing device 17; a hollow-core optical fiber 18; a vacuum pump 19.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1, the present invention provides a fiber raman spectroscopy gas analysis apparatus, comprising: the device comprises a laser 1, a light beam coupling device, a gas sample chamber 4, a collimation and beam splitting device and a photoelectric imaging receiving device; the light beam coupling device is used for coupling laser emitted by the laser 1 into the gas sample chamber; the gas sample chamber 4 is used for enabling the coupled laser to act with gas molecules to be detected in a hollow optical fiber core 18 of the gas sample chamber 4 to generate Raman scattering, and transmitting a mixed beam of a forward scattering signal and the laser to the collimation beam splitting device; the collimation beam splitting device is used for collimating the mixed light beam, separating laser in the mixed light beam, and transmitting the light beam only containing the forward scattering signal to the photoelectric imaging receiving device; and the photoelectric imaging receiving device is used for collecting the forward scattering signals and carrying out digital spatial filtering on the forward scattering signals to obtain the Raman spectrum of the gas to be detected.
In one embodiment of the invention, the laser adopted by the invention is a narrow linewidth laser of 532nm, the continuous output power can reach 200mW and the beam quality factor M can be considered in consideration of the volume and the cost of equipment2Less than 1.2, can pass through the focusing coupling lens 3 and the hollow-core optical fiber 18The guided modes are well matched. The power of the laser and the intensity of Raman scattering are in a linear relation, and the higher the power is, the higher the Raman scattering intensity is.
To explain further, the light beam coupling device comprises a laser line filter 2 and a focusing coupling lens 3; the laser line filter 2 is used for filtering fluorescent components in the laser generated by the laser 1; the focusing coupling lens 3 is used for converging the laser light and coupling the laser light into the hollow-core optical fiber 18. As shown in fig. 1, in an embodiment of the present invention, the focusing coupling lens 3 has a focal length of 60mm, the laser generated by the laser 1 filters fluorescent components generated by optical elements such as a laser gain medium or a window through the laser line filter 2, the focusing coupling lens 3 converges the laser to match the numerical aperture of the hollow-core optical fiber 18, and the laser is efficiently coupled into the hollow-core optical fiber 18, so that the laser in the hollow-core optical fiber 18 interacts with molecules of a gas to be detected to generate raman scattering.
To explain further, the gas sample chamber 4 comprises a gas storage bottle 13, a pipeline 14, an electromagnetic valve 15, a gas pressure gauge 16, a hollow optical fiber 18, a fixing device 17 and a vacuum pump 19; the gas storage bottle 13 is used for storing the gas to be detected; the hollow-core optical fiber 18 is used for enabling the gas to be detected to act with laser to generate Raman scattering; the fixing device 17 is used for fixing two ends of the hollow-core optical fiber 18; the vacuum pump 19 is used for evacuating the gas in the hollow-core optical fiber 18 when the gas to be measured is updated; the gas storage bottle 13 is connected with the hollow-core optical fiber 18 through the pipeline 14, the hollow-core optical fiber 18 is connected with the vacuum pump 19 through the pipeline 14, and the pipeline 14 is used for conveying the gas to be detected. In the embodiment of the gas sample chamber 4 of the present invention shown in fig. 2, the gas to be measured in the gas bomb 13 can be filled into the hollow-core optical fiber 18 through the pipeline 14, the electromagnetic valve 15 controls the on-off of the gas path to realize the rapid change of the gas pressure and the gas type in the hollow-core optical fiber 18, and the barometer 16 is used for indicating the gas pressure. The fixing device 17 with an optical window is installed at both ends of the hollow-core optical fiber 18, and when gas is refreshed, the vacuum pump 19 evacuates the gas in the hollow-core optical fiber 18. It should be noted that, in order to achieve a compact device structure, the hollow-core optical fiber 18 may be wound into a circular ring having a radius of not less than 10 cm.
In a further elaboration, the hollow-core optical fibre 18 is a hypocycloid-type Kagomse hollow-core optical fibre. The invention selects the hollow-core optical fiber for inhibiting the coupling light guide mechanism and the hypocycloid Kagomse hollow-core optical fiber as the preferred embodiment of the invention, the cladding of the optical fiber is of a large-spacing Kagomse lattice structure, and the core is of a hypocycloid shape. The fiber structure can inhibit the coupling of a fiber core conduction mode to a cladding, the fiber core mode and the cladding mode are only overlapped in a small amount of space, the Raman/fluorescence background excited by the cladding mode is weak, and the background of the obtained spectrum is relatively flat. When the length of the optical fiber is less than the attenuation length (the reciprocal of the attenuation coefficient) of the optical fiber, the forward Raman scattering intensity is equivalent to the backward Raman scattering intensity. The signal still has the influence of Raman/fluorescence background generated by a small number of cladding modes, and the digital spatial filtering can further reduce the background. The general spatial filter consists of a convergent lens, a spatial diaphragm at a focus and a collimating lens, the difficulty of adjusting a light path is increased, the shape and the position of the spatial diaphragm are not necessarily consistent with a Raman scattering light spot generated by a conduction mode, and the device stability is highly required.
To explain further, the collimation and beam splitting device comprises a collimation lens 5, a dichroic mirror 6, a light beam blocking device 7 and a long-pass filter 8; the collimating lens 5 is used for changing the mixed light beam output by the gas sample chamber 4 into a collimated parallel light beam; the dichroic mirror 6 is used for separating laser light in the mixed light beam from a forward scattering signal; the beam blocking device 7 is used for absorbing the laser light in the mixed beam reflected by the dichroic mirror 6; the long-pass filter 8 is used for filtering residual laser in the forward scattering signal to obtain a light beam only containing the scattering signal. It should be noted that the focal length of the collimating lens 5 is 40mm, as shown in fig. 1, the device collects raman scattering signals by using a forward scattering structure, a mixed beam of the raman scattering signals and laser light is collimated by the collimating lens 5 and then substantially separated by the dichroic mirror 6, and the transmitted laser light is blocked and absorbed by the beam blocking device 7. The transmitted mixed beam passes through the long pass filter 8 to filter out residual laser light.
In a further description, the optoelectronic imaging receiving device comprises an optical radiation collecting lens 9, a spectrometer 10, a detector 11 and a data processing device 12; the spectrometer 10 is used for obtaining the spectral distribution of the forward scattering signal which is collected by the optical radiation collecting lens 9 and passes through the long pass filter 8; the detector 11 is used for imaging the spectral distribution of the forward scatter signal; the data output end of the detector 11 is connected to the data processing device 12, and the data processing device 12 is configured to control the acquisition and processing of the forward scattering signal, implement digital spatial filtering, and obtain a raman spectrum of the gas to be detected. As shown in fig. 1, in an embodiment of the present invention, an optical radiation collecting lens 9 of the spectrometer 10 collects a forward scattering signal, and finally images the forward scattering signal onto the detector 11, a data output end of the detector 11 is connected to the computer 12, and the acquisition and processing of the signal are controlled by software, and in an image mode, the optical radiation collecting lens 9 is adjusted to clearly converge the collected raman scattering signal of the gas to be measured in the hollow-core optical fiber 18 onto the detector 11, and then digital spatial filtering and data acquisition are performed. The data processing device 12 in the present invention is a computer. And analyzing the collected low background Raman spectrum to obtain the components of the gas to be detected. In contrast, the device adopts a digital spatial filtering method of the imaging spectrometer, can realize automatic focusing of the spectrometer and automatic selection of a spectrum integration region through control software of the CCD array detector, reduces Raman/fluorescence background generated by a cladding mode, simplifies an experimental device and is convenient for experimental operation. For the detection of trace gas, the background in the Raman spectrum is easy to annihilate weak signals, and the hollow fiber selected by the invention has low fiber core mode/cladding mode space overlapping rate. It should be noted that the transmission band of the hollow-core optical fiber is 500-700nm, and under 532nm laser excitation, the corresponding Stokes Raman shift range is 0-4511 cm-1Almost all places including hydrogen can be collected at the same timeA Raman signal having a gas-based vibrational band; the diameter of the fiber core is 30 +/-1 mu m, which is several times larger than that of the fiber core of the band gap type hollow photonic crystal fiber, so that the gas can be conveniently updated, and the rapid on-line detection can be realized; the transmission loss of 532nm laser is 30dB/km +/-10, and the length of the optical fiber is 2 m.
Stated further, the data processing device 12 is also used to adjust the focus of the optical radiation collection lens 9 so that the forward scatter signal is clearly focused on the detector 11.
In further illustration, the detector 11 is a CCD array detector. It should be noted that the CCD array detector has two modes, namely an image mode and a spectrum mode, and the optical radiation collecting lens 8 can be adjusted by using the image mode, so that the raman scattering generated by the gas sample to be measured in the hollow optical fiber 18 can be clearly imaged on the CCD array detector, and a pixel row corresponding to a raman scattering signal generated by the hollow optical fiber conducting mode is selected for integration according to the result of the image mode, thereby preventing the raman/fluorescence radiation generated by the cladding mode from increasing the signal background. The CCD digital spatial filtering of the forward Raman scattering collection integrated imaging spectrometer can obviously reduce the Raman/fluorescence background of the spectrum signal, improve the signal-to-noise ratio of the device and provide favorable support for the detection of the trace component gas. The imaging spectrometer digital spatial filtering adopted by the device is compared with a pinhole component spatial filter, so that the experimental device is further simplified, and the difficulty in light path adjustment is reduced.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A fiber raman spectroscopy gas analysis apparatus, comprising: the device comprises a laser, a light beam coupling device, a gas sample chamber, a collimation and beam splitting device and a photoelectric imaging receiving device;
the light beam coupling device is used for coupling laser emitted by the laser into the gas sample chamber;
the gas sample chamber is used for enabling the coupled laser to act with gas molecules to be detected in a hollow optical fiber core of the gas sample chamber to generate Raman scattering, and transmitting a mixed beam of a forward scattering signal and the laser to the collimation beam splitting device;
the collimation beam splitting device is used for collimating the mixed light beam, separating laser in the mixed light beam, and transmitting the light beam only containing the forward scattering signal to the photoelectric imaging receiving device;
and the photoelectric imaging receiving device is used for collecting the forward scattering signals and carrying out digital spatial filtering on the forward scattering signals to obtain the Raman spectrum of the gas to be detected.
2. The fiber raman spectroscopy gas analysis apparatus of claim 1, wherein: the light beam coupling device comprises a laser line filter and a focusing coupling lens; the laser line filter is used for filtering fluorescent components in laser generated by the laser; the focusing coupling lens is used for converging the laser and coupling the laser into the hollow-core optical fiber.
3. The fiber raman spectroscopy gas analysis apparatus of claim 1, wherein: the gas sample chamber comprises a gas storage bottle, a pipeline, a hollow optical fiber, a fixing device and a vacuum pump;
the gas storage bottle is used for storing the gas to be detected; the hollow optical fiber is used for enabling the gas to be detected to act with laser to generate Raman scattering; the fixing device is used for fixing two ends of the hollow optical fiber; the vacuum pump is used for evacuating the gas in the hollow-core optical fiber when the gas to be detected is updated; the gas storage bottle is connected with the hollow optical fiber through the pipeline, the hollow optical fiber is connected with the vacuum pump through the pipeline, and the pipeline is used for conveying the gas to be detected.
4. The fiber Raman spectroscopy gas analysis apparatus of claim 3, wherein: the gas sample cell further comprises a solenoid valve; the electromagnetic valve is arranged between the gas storage bottle and the hollow optical fiber and used for controlling the on-off of the gas path.
5. The fiber Raman spectroscopy gas analysis apparatus of claim 4, wherein: the gas sample chamber further comprises a barometer; the barometer is arranged between the electromagnetic valve and the hollow-core optical fiber and used for displaying the air pressure of the gas to be detected in the pipeline.
6. The fiber Raman spectroscopy gas analysis apparatus of claim 3, wherein: the hollow-core optical fiber is a hypocycloid Kagomse hollow-core optical fiber.
7. The fiber raman spectroscopy gas analysis apparatus of claim 1, wherein: the collimation beam splitting device comprises a collimation lens, a dichroic mirror, a light beam blocking device and a long-pass filter plate;
the collimating lens is used for converting the mixed light beam output by the gas sample chamber into a collimated parallel light beam; the dichroic mirror is used for separating laser light in the mixed light beam from a forward scattering signal; the beam blocking device is used for absorbing laser in the mixed beam reflected by the dichroic mirror; the long-pass filter is used for filtering residual laser in the forward scattering signals to obtain light beams only containing scattering signals.
8. The fiber raman spectroscopy gas analysis apparatus of claim 7, wherein: the photoelectric imaging receiving device comprises an optical radiation collecting lens, a spectrometer, a detector and a data processing device;
the spectrometer is used for obtaining the spectral distribution of the forward scattering signals which are collected by the optical radiation collecting lens and penetrate through the long-pass filter; the detector is used for imaging the spectral distribution of the forward scattering signal; and the data output end of the detector is connected with the data processing device, and the data processing device is used for controlling the acquisition and processing of the forward scattering signal, implementing digital spatial filtering and obtaining the Raman spectrum of the gas to be detected.
9. The fiber raman spectroscopy gas analysis apparatus of claim 8, wherein: the data processing device is also used for adjusting the focusing of the optical radiation collecting lens so as to lead the forward scattering signals to be converged on the detector.
10. The fiber raman spectroscopy gas analysis apparatus of claim 8, wherein: the detector is a CCD array detector.
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