CN110849838A - Multi-component gas detection method and device based on silicon-based integrated hollow-core optical waveguide - Google Patents
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Abstract
The invention discloses a multi-component gas detection method and a device based on a silicon-based integrated hollow-core optical waveguide, which comprises the following steps: light is emitted from a broadband light source, and is introduced into the silicon-based iHWG of the closed space through an optical fiber; the gas to be detected enters the silicon-based iHGW hollow channel with the hole in a diffusion mode; when infrared light with a certain wavelength passes through the gas to be detected, the concentration change of the gas to be detected causes the light intensity of the characteristic wavelength of the characteristic absorption peak of the gas to be detected to change; the infrared spectrum and the data of the standard spectrum library are compared and analyzed by the aid of the Lambert-beer law to obtain the concentration of the to-be-detected multi-component gas, and type judgment and concentration measurement of the target gas can be achieved. The invention ensures the long-term stable work of the system under the complex conditions of sealing, temperature and humidity change, radiation and external vibration, and realizes the calibration-free detection of other types of gases with characteristic absorption peaks in the wavelength range covered by the measured gas in the sealed space.
Description
Technical Field
The invention relates to long-term online high-precision detection of multi-component gas, belonging to the technical field of hollow optical waveguide gas detection.
Background
Hollow-core optical waveguides (HWGs, also known as hollow-core fibers) are typically a type of waveguide used for optical transmission with a central hole surrounded by a highly reflective inner wall. HWG has several advantages over traditional solid optical fibers: the transmission band range is wide (0.9-25 mu m), high-power laser (with high laser power damage threshold) can be transmitted, the structure is relatively simple, the cost is potentially low, the nonlinear effect is low, the insertion loss is low (no Fresnel reflection exists on the end face of the HWG when light is coupled into the hollow-core optical waveguide from free space), no end face reflection exists, the light beam divergence angle is small, the optical waveguide material does not selectively absorb interference, and the like.
The hollow optical waveguide is used in spectrum gas detection, can realize the transmission of an optical path, and can also be used as a gas sample pool to realize the long-optical-path high-sensitivity measurement function. Compared with the traditional multi-reflection gas sample cell, the advantages of the multi-reflection gas sample cell include the following aspects: (1) the volume is small, usually in the order of mL, and the response time can be faster; (2) the gas path and the light path are transmitted in the device simultaneously, so that the cost is relatively low; (3) the flexibility of the hollow-core optical waveguide enables the sensor to be easily miniaturized and suitable for field application. In addition, the low-loss transmission in near infrared and middle infrared bands can be realized, and the gas sample cell can be used in Fourier transform infrared spectroscopy (FTIR), Tunable Laser Absorption Spectroscopy (TLAS) and other spectral measurement systems to realize applications such as atmospheric environment monitoring and respiratory gas diagnosis.
At present, three hollow core optical waveguides commonly used in spectral gas-sensitive detection are available, namely traditional SiO2Plating Ag/AgI hollow core optical waveguide (Ag/AgI-HWG) on the tube; photonic band gap hollow core optical waveguides (PBG-HWG) and substrate integrated hollow core optical waveguides (iHWG). The substrate integrated hollow-core optical waveguide refers to planar hollow-core optical waveguide, and mainly comprises a substrate, an optical waveguide structure layer and a top layer. There are many choices for the substrate, optical waveguide and top plate materials, wherein the hollow core structure of the optical waveguide must ensure a sufficiently long gas absorption length, be capable of being integrated with a light source, a detector, etc., and be capable of absorbing wavelength light fluxWhen the waveguide structure is passed, the loss amount is small. With the increasing requirements on the aspects of the volume of a detection system, the convenience of a coupling element and the like, the research on the substrate integrated hollow-core optical waveguide device is more and more concerned, and the application of the substrate integrated hollow-core optical waveguide device in a biochemical sensor is more and more deep.
Disclosure of Invention
The invention provides a gas detection method based on a silicon-based integrated hollow-core optical waveguide (Si-iHWG), aiming at a series of requirements of high precision, low detection limit, multi-component, high selectivity, on-line property, long service life, no calibration, small volume, safety and the like in the detection of multi-component gas in a closed space.
The invention is realized by the following technical scheme.
The invention provides a multi-component gas detection method based on a silicon-based integrated hollow-core optical waveguide, which comprises the following steps:
a. light emitted by the broadband light source passes through the standard absorber and is introduced into a detection light channel and a reference light channel of the silicon-based iHWG in the closed space through the optical fiber;
b. the multi-component gas to be detected enters a detection light channel of the silicon-based iHWG in a free diffusion mode through a gas diffusion channel of the silicon-based iHWG;
c. when infrared light with a certain wavelength passes through the multi-component gas to be detected, due to the absorption effect of the gas, the concentration change of the multi-component gas to be detected causes the light intensity of the characteristic wavelength of the characteristic absorption peak of the multi-component gas to be detected to change, the infrared spectrum with the changed light intensity is transmitted to the detector through the emergent optical fiber, and the infrared spectrum is obtained by the control device;
d. the control device compares and analyzes the infrared spectrum and the data of the standard spectrum library, and the concentration of the multi-component gas to be detected is obtained through the Lambert-beer law; the type judgment and the concentration measurement of the multi-component gas to be measured can be realized.
In the scheme, the concentration calculation method of the multi-component gas to be measured is obtained according to the Lambert-beer law, and the concentration calculation method is based on the intensity I of transmitted light and the intensity I of incident light0The ratio of the transmittance is referred to as the transmittance T, and the log (1/T) which is the logarithmic value A of the reciprocal of the transmittance is obtained.
In the above scheme, the total absorbance at any wavenumber can be obtained for a multi-component gas if each component obeys lambert-beer's law.
The invention correspondingly provides a multi-component gas detection system based on a silicon-based integrated hollow-core optical waveguide, which comprises a broadband light source, a standard absorber, an optical fiber connector, a silicon-based iHWG, a detector and a control device; the broadband light source, the standard absorber, the optical fiber connector and the silicon-based iHWG are sequentially connected through an incident optical fiber to form an incident light channel; and the silicon-based iHWG, the optical fiber connector and the standard absorber are respectively and sequentially connected with the detector and the control device through the emergent optical fiber to form an emergent light channel.
In the above scheme, the silicon-based iHWG comprises lower cladding silicon and upper cladding glass, wherein a detection light channel and a reference light channel are etched on the lower cladding silicon, and a gas diffusion channel corresponding to the detection light channel is arranged on the upper cladding glass; an incident optical fiber and an exit optical fiber are respectively introduced into the detection light channel and the reference light channel.
In the above scheme, the detection light channel is etched at the periphery of the reference light channel.
In the above scheme, the gas diffusion channel is a plurality of through holes corresponding to the detection light channel.
The multi-component gas detection based on the silicon-based integrated hollow-core optical waveguide can be applied to atmosphere detection of a closed space of a high-precision inertial navigation element or a propeller, and particularly to the accurate online detection of the multi-component gas.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the device ensures the long-term stable work of the system under the complex conditions of sealing, temperature and humidity change, radiation and external vibration, and realizes H in the sealed space2、O2、H2O、CO2、CxHy、NxOyAnd other types of gases having characteristic absorption peaks in the wavelength range covered by these gases under test. The sensitive part of the device is a silicon-based iHWG, and is connected with an external light source and a detection system through optical fibers, so that the tightness of a detection space is ensured. Silicon-based light waveThe diffusion type gas absorption cavity is adopted for guiding, the side wall of the optical channel is subjected to dry deep silicon etching, and then a reflective film is deposited to reduce the roughness and the optical loss. And a light path differential structure is designed, and a differential spectrum algorithm is used, so that cross interference is eliminated, and high-precision multi-component gas detection is realized. The in-situ online calibration method for comparing the internal absorption spectrum with the external standard absorption cavity as a reference avoids the system precision exceeding a preset range, so that the detection system works for a long time.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention:
FIG. 1 is a schematic diagram of a silicon-based iHWG-based fiber-coupled multi-component gas detection system according to the present invention.
Fig. 2 is a schematic representation of the light passing through a silicon-based iHWG of the present invention.
FIG. 3 is a schematic diagram of a silicon-based iHWG absorption cavity, sidewalls and a highly reflective film of the present invention, wherein A is the sidewalls and B is the highly reflective film.
Fig. 4 is a schematic diagram of a silicon-based iHWG process of the present invention.
FIG. 5, FIG. 6, FIG. 7, FIG. 8, FIG. 9, FIG. 10 and FIG. 11 are each H2O、O2、H2、O2、NO2、NO、CH4Absorption spectra in the mid-infrared range (WN ═ 500-.
In the figure: 1, a broadband light source; 2, a standard absorber; 3, an optical fiber; 4, an optical fiber joint; 5, silicon-based iHWG; 6, a detector; 7, a control device; 8, upper cladding glass; 9, lower cladding silicon; 10, detecting a light channel; 11, gas diffusion channels; 12, a reference light channel; 13. 14, inner and outer incident optical fibers; 15. 16, outer and inner outgoing optical fibers; and 17, sealing the space.
Detailed Description
The present invention will now be described in detail with reference to the drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the present invention are provided to explain the present invention without limiting the invention thereto.
Fig. 1 is a schematic diagram of a silicon-based iHWG-based fiber-coupled multi-component gas detection system. The method comprises the following steps: the device comprises a broadband light source 1, a standard absorber 2, an optical fiber 3, an optical fiber joint 4, a silicon-based iHWG 5, a detector 6, a control device 7 and a closed space 17. The broadband light source 1, the standard absorber 2, the optical fiber connector 4 and the silicon-based iHWG 5 are sequentially connected through the incident optical fiber 3 to form an incident light channel; the silica-based iHWG 5, the optical fiber connector 4 and the standard absorber 2 are respectively connected with the detector 6 and the control device 7 in sequence through the emergent optical fiber 3 to form an emergent light channel.
Fig. 2 is a schematic diagram of light passing through a silicon-based ihhg. The method comprises the following steps: the light detection device comprises upper cladding glass 8 and lower cladding silicon 9, wherein a detection light channel 10 and a reference light channel 12 are etched on the lower cladding silicon 9, and the detection light channel 10 is etched on the periphery of the reference light channel 12. The upper cladding glass 8 is provided with a gas diffusion channel 11 corresponding to the detection light channel 10; the detection light channel 10 and the reference light channel 12 are respectively introduced with inner and outer incident optical fibers 13, 14 and inner and outer emergent optical fibers 15, 16, the incident optical fibers 13, 14 respectively transmit light to the detection light channel 10 and the reference light channel 12, the measured multi-component gas enters the detection light channel 10 in a diffusion mode, and finally, light signals are output through the outer and inner emergent optical fibers 15, 16.
As shown in fig. 3, the structure and process of the silicon-based iHGW 5 are shown, wherein a is the sidewall of the detection light channel 10 and the reference light channel 12, and B is the highly reflective film of the sidewall of the detection light channel 10 and the reference light channel 12. Through the optimization of deep silicon etching process parameters, the detection light channel 10 and the reference light channel 12 with high dimensional accuracy are processed, so that the side walls of the detection light channel 10 and the reference light channel 12 have good steepness and low surface roughness, and the accurate coupling with optical fibers and the low-loss transmission of infrared light in the hollow optical waveguide are ensured. The etching process is shown in fig. 4.
The process of detecting the multi-component gas in the closed chamber by using the device is as follows:
a. light is emitted from a broadband light source 1, passes through a standard absorber 2, and is introduced into a silicon-based iHWG 5 of an enclosed space 17 through an optical fiber 3. The silicon-based iHWG 5 is characterized as follows, see fig. 2:
the silicon-based iHGW 5 is fabricated as a 2-layer layered structure based on a modular concept. Aiming at the detection of multi-component gas in a closed space, a silicon-based iHWG 5 adopts a diffusion type gas absorption cavity, and a deposition method of a high-reflection film with better flexibility is selected for the lower cladding silicon 9 to carry out dry deep silicon etching processing on a waveguide layer, namely a detection light channel 10 and a reference light channel 12, so that the absorption micro-channels of the bottom surface and the side surface with low roughness and good planeness are realized, and the light loss is reduced.
An optical path differential structure is designed on the silicon-based iHGW 5, namely a detection optical channel 10 and a reference optical channel 12 are etched, so that the purpose of eliminating environmental interference by using a differential spectrum algorithm and realizing high-precision multi-component gas detection is achieved.
A plurality of gas diffusion channels 11 corresponding to the detection light channels 10 are processed on the upper cladding glass 8.
b. The multi-component gas to be detected enters the detection light channel 10 through the gas diffusion channel 11 in a free diffusion mode;
c. when infrared light with a certain wavelength passes through the multi-component gas to be detected, the concentration change of the multi-component gas to be detected causes the light intensity of the characteristic wavelength of the characteristic absorption peak to change due to the absorption effect of the gas; the infrared spectrum with the changed light intensity is transmitted to a detector through the internal and external light fibers 15 and 16, and the infrared spectrum is obtained by a control device;
d. the control device compares and analyzes the infrared spectrum and the data of the standard spectrum library, and the concentration of the multi-component gas to be detected is obtained through the Lambert-beer law; the type judgment and the concentration measurement of the multi-component gas to be measured can be realized.
For the detection process, the absorption of the gas can be obtained from the lambert-beer law:
intensity of transmitted light I and intensity of incident light I0The ratio of (A) to (B), referred to as the transmittance, is represented by T and is not more than 1. Log (1/T), the log of the reciprocal transmission, is expressed as a:
wherein T represents transmittance, a(v)Is the molar absorbance coefficient, which is related to the nature of the absorbing species and the wave number v of the incident light, and b is the thickness of the absorbing layercm, c is the concentration of the light-absorbing substance in mol. L-1。
For multi-component mixtures, the additivity of lambert-beer law applies. If each component obeys Lambert-beer's law, then the total absorbance at any wavenumber is given by:
wherein A (i) is the total absorbance of the plurality of components at the i-th wavenumber, aijIs the absorption coefficient of the jth component at the ith wavenumber; b is the sample cell thickness; c. CjIs the concentration of the jth component.
FIGS. 5-11 show H, respectively2O、O2、H2、CO2、NO2、NO、CH4In the absorption standard spectrogram in the middle infrared incident light range (WN ═ 500-4000/cm), the invention compares the obtained detection spectrum with the standard spectrogram according to the change of the light intensity of the characteristic wavelength of the characteristic absorption peak of the detected gas caused by the change of the concentration of the detected gas, thereby carrying out the type judgment and the concentration measurement of the gas.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (8)
1. A multi-component gas detection method based on a silicon-based integrated hollow-core optical waveguide is characterized by comprising the following steps:
a. light emitted by the broadband light source passes through the standard absorber and is introduced into a detection light channel and a reference light channel of the silicon-based iHWG in the closed space through the optical fiber;
b. the multi-component gas to be detected enters a detection light channel of the silicon-based iHWG in a free diffusion mode through a gas diffusion channel of the silicon-based iHWG;
c. when infrared light with a certain wavelength passes through the multi-component gas to be detected, due to the absorption effect of the gas, the concentration change of the multi-component gas to be detected causes the light intensity of the characteristic wavelength of the characteristic absorption peak of the multi-component gas to be detected to change, the infrared spectrum with the changed light intensity is transmitted to the detector through the emergent optical fiber, and the infrared spectrum is obtained by the control device;
d. the control device compares and analyzes the infrared spectrum and the data of the standard spectrum library, and the concentration of the multi-component gas to be detected is obtained through the Lambert-beer law; the type judgment and the concentration measurement of the multi-component gas to be measured can be realized.
2. The method for detecting the multi-component gas based on the silicon-based integrated hollow-core optical waveguide according to claim 1, wherein the method for calculating the concentration of the multi-component gas to be detected according to the Lambert-beer law is as follows:
intensity of transmitted light I and intensity of incident light I0The ratio is called the transmittance T, and the log (1/T) which is the logarithmic value A of the reciprocal of the transmittance:
wherein, a(v)The molar absorbance coefficient, b the thickness of the absorbing layer, and c the concentration of the light absorbing substance.
3. The method according to claim 1, wherein if each component of the multi-component gas complies with the lambert-beer law, the total absorbance at any wavenumber is given by the following formula:
wherein A (i) is the total absorbance of the plurality of components at the i-th wavenumber, aijIs the absorption coefficient of the jth component at the ith wavenumber; b is the sample cell thickness; c. CjIs the concentration of the jth component.
4. A multi-component gas detection system based on a silicon-based integrated hollow-core optical waveguide is characterized by comprising a broadband light source, a standard absorber, an optical fiber connector, a silicon-based iHWG, a detector and a control device; the broadband light source, the standard absorber, the optical fiber connector and the silicon-based iHWG are sequentially connected through an incident optical fiber to form an incident light channel; and the silicon-based iHWG, the optical fiber connector and the standard absorber are respectively and sequentially connected with the detector and the control device through the emergent optical fiber to form an emergent light channel.
5. The system according to claim 4, wherein the silicon-based iHWG comprises a lower cladding silicon and an upper cladding glass, a detection light channel and a reference light channel are etched on the lower cladding silicon, and a gas diffusion channel corresponding to the detection light channel is arranged on the upper cladding glass; an incident optical fiber and an exit optical fiber are respectively introduced into the detection light channel and the reference light channel.
6. The silicon-based integrated hollow-core optical waveguide-based multi-component gas detection system according to claim 5, wherein the detection light channel is etched at the periphery of the reference light channel.
7. The silicon-based integrated hollow-core optical waveguide-based multi-component gas detection system according to claim 5, wherein the gas diffusion channel is a plurality of through holes corresponding to the detection light channel.
8. The multi-component gas detection based on the silicon-based integrated hollow-core optical waveguide can be applied to atmosphere detection of a closed space of a high-precision inertial navigation element or a propeller, and particularly can be used for accurate online detection of the multi-component gas.
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| CN113155760A (en) * | 2021-04-02 | 2021-07-23 | 宁波大学 | Spectrophotometric detection sensor |
| CN113155760B (en) * | 2021-04-02 | 2022-11-15 | 宁波大学 | Spectrophotometric detection sensor |
| CN116297279A (en) * | 2023-05-18 | 2023-06-23 | 至芯半导体(杭州)有限公司 | Method, system, device and equipment for detecting concentration of formaldehyde gas/VOC gas |
| CN116297279B (en) * | 2023-05-18 | 2023-12-19 | 至芯半导体(杭州)有限公司 | Method, system, device and equipment for detecting concentration of formaldehyde gas/VOC gas |
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