CN102590112B - Surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas detection method and device - Google Patents
Surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas detection method and device Download PDFInfo
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Abstract
The invention relates to a surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas detection method and device. The device comprises a tunable laser, a reflective object, a surface microstructure silicon cantilever, a concave mirror, an optical fiber, an optical fiber coupler, a continuous laser, a laser controller, an optical detector, a signal processing system and the like. Modulated light emitted from the tunable laser is reflected on the concave mirror by the reflective object after passing through the gas to be detected, the received reflective light on the concave mirror is focused on a silicon surface of the cantilever beam. After the optical energy is absorbed by the cantilever beam, the optical-thermal deflection occurs to generate resonance. If the gas concentration is higher, the optical intensity absorbed by the gas is larger, and if the optical energy absorbed by the cantilever beam is smaller and the resonance amplitude is smaller. A length adjustable Fabry-Perot cavity is formed by an optical fiber end surface and a metal surface of the cantilever beam, the amplitude of the cantilever beam is demodulated to obtain gas absorption spectrum, furthermore the concentration of the detected trace gas is obtained. The device has the advantages of cheap price, small size, simple structure, convenience in use, strong flexibility, high detection sensitivity, and field work capacity and can be widely used in remotely detecting the components and concentration of a variety of or multi-component trace gas.
Description
Technical field
The present invention relates to the detection of gas technology, especially a kind of photothermal spectroscopy trace gas detection method and device that trace gas is carried out to long-range detection based on the surface micro-structure silicon cantilever of working under open environment, can be widely used in the fields such as long-distance explosive detection, environmental monitoring and the detection of poisonous and harmful hazardous gas.
Background technology
The development of trace gas remote probing techniques is for atmosphere environment supervision, and the long-range detection of explosive and biological physiology state-detection etc. all tool are of great significance.It is large that the absorption spectrum gas detection technology has measurement range, but measurement of multi-components, but the advantages such as continuous monitoring become desirable trace gas concentration testing tool gradually.The absorption spectrum gas detection technology mainly comprises difference absorption spectrum technology, tunable laser diodes absorption spectroscopy techniques, laser Induced Fluorescence Technology and optoacoustic spectroscopy etc.The characteristics such as wherein, optoacoustic spectroscopy is highly sensitive owing to having, and antijamming capability is strong, dynamic range is large, and explorer response and incident wavelength are irrelevant are all one of most important developing direction of Trace gas detection technology all the time.
In order to improve the detection sensitivity of optoacoustic spectroscopy, people are devoted to improve the structure of photoacoustic cell always and adopt sensitiveer microphone etc. to improve this technology of development.For example 2002, the optoacoustic spectroscopy group of Holland Nijmegen university utilizes the optoacoustic spectroscopy system that optical parametric oscillator is built that the detection sensitivity of ethane is brought up to the 10ppt level, Anbui Optical Machinery Inst., Chinese Academy of Sciences in 2009 have proposed a kind of device of the quartz tuning fork strengthened optoacoustic spectroscopy gas based on acoustic resonance cavity, and measure in real time the water vapor concentration under atmospheric pressure, it surveys the normalization equivalent noise is 5.9 * 10
-10Cm
-1W/Hz
1/2.The people such as Finland V.KOSKINEN have proposed a kind of " the optoacoustic spectroscopy sniffer strengthened based on semi-girder ", have surveyed the concentration of carbon dioxide, and it surveys the normalization equivalent noise is 1.7 * 10
-10Cm
-1W/Hz
1/2.Although these class methods have very high detection sensitivity, due to the use of photoacoustic cell, limited the method and only can have been surveyed in the trace gas domain of the existence, and can not carry out long-range detection.Thereby be subject to greatly restriction in the application that the hazardous gas such as poisonous, inflammable and explosive is surveyed.
In order to overcome above-mentioned deficiency, realize adopting the optoacoustic spectroscopy method to realize long-range detection to trace gas, under USDOE, Oak Ridge National Laboratory proposed a kind of detection system of the optoacoustic spectroscopy for the long-range detection explosive in 2008.In this system, the Ear Mucosa Treated by He Ne Laser Irradiation that the quantum laser device sends is detected thing by being focused on quartz tuning-fork after concave mirror by baffle reflection to the 20m place, thereby causes tuning fork vibration.Due to the piezoelectric effect of tuning fork, the quartz tuning-fork of vibration will produce the piezoelectric current signal, and this signal carries out demodulation through lock-in amplifier at the resonance frequency place, thereby obtain the absorption spectra of gaseous sample.But this detection method adopts quartz tuning-fork to absorb device as luminous energy, and its absorptance is lower, thereby has limited the further raising of detection sensitivity.In addition, if improve the detection sensitivity of tuning fork, need larger laser energy, thereby greatly increased the risk that flammable explosive gas is surveyed.Afterwards, this laboratory proposes again a kind of Explosives Detection System based on semi-girder, can realize the detection of three kinds of typical explosives in 1 meter scope, compares quartzy enhanced photo acoustic spectrum investigating system, and this system has higher detection accuracy.But, because this silicon nitride cantilevers beam is very low to the absorption efficiency of incident light, greatly reduced its ability that faint optical signal is surveyed, thereby can't carry out remote spectrographic detection; And this flexibility of cantilever is lower, the thermal deflection inefficiency, therefore need to adopt expensive high precision position sensitive detection system to pick up the vibration amplitude of semi-girder, causes the system architecture complexity, expensive.
Summary of the invention
The object of the invention is to overcome weak point of the prior art, a kind of photothermal spectroscopy detection method and device based on the surface micro-structure silicon cantilever of surveying for trace gas under open environment proposed, a kind of cheapness, volume is little, simple in structure, easy to use, detection sensitivity is high, possess the field environment ability to work, can be for long-range detection method and the device of multiple or polycomponent trace gas.
For solving technical matters of the present invention, the technical scheme adopted is:
A kind of surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas detection method, described method is to allow the pulse laser sent from tunable laser pass through detected gas, after being absorbed, incide on reflecting object, process reflecting object back reflection is to concave mirror, with concave mirror, the luminous energy received is focused on the surface micro-structure silicon cantilever, after absorbing luminous energy by the surface micro-structure silicon cantilever, resonance occurs, the tunable Fabry-perot optical fiber demodulating system simultaneously formed by the metal surface based on fiber end face and semi-girder is picked up the vibration signal of this surface micro-structure silicon cantilever, when semi-girder generation resonance, the chamber length of Fa-Po cavity changes, thereby cause the variation of reflection interference light intensity generating period, obtain the resonance signal of semi-girder by the intensity demodulation to this light signal, finally adopt signal processing system to be finally inversed by the concentration that is detected gas.
Realize the photothermal spectroscopy trace gas sniffer based on the surface micro-structure silicon cantilever of said method, it comprises tunable laser, reflecting object, surface micro-structure silicon cantilever, concave mirror, optical fiber, fiber coupler, continuous wave laser, single-point photodetector, signal processing system, optical fiber, optical fiber and laser controller.
Described surface micro-structure silicon cantilever is double-decker, and upper strata (being light-absorption layer) is surface micro-structure silicon.It is that the method that adds the sulfur hexafluoride etchant gas with femto-second laser pulse goes out a plurality of micro-cone structures in this surface etch, the element sulphur concentration that adopts pressure to mix surface micro-structure silicon at 60Kpa to the method increase of concentration of sulfur hexafluoride corrosion between 80Kpa, thereby changed the band structure of surface micro-structure silicon, and then improved semi-girder and arrived the extinction efficiency of infrared band in ultraviolet, and more smooth at this wavelength band internal absorptance, realized that the non-selectivity to the infrared full-wave section absorbs to ultraviolet, laser wavelength is had to the non-selectivity absorption characteristic, can meet the requirement of wide spectrographic detection, can survey multiple trace gas or organize the concentration that trace divides gas more.
This structure can greatly improve being detected the absorption efficiency of laser, and the photo-thermal conversion coefficient of structure is increased greatly, and under equal exciting light energy, the semi-girder vibration amplitude enlarges markedly, thereby greatly improves the detection sensitivity of system.Upper surface microstructure silicon thickness is the 2.5-28 micron, and the micro-cone surface structure is micron and nano-scale, is " pyramid " type, and the ratio of cone height and bottom surface diameter is between 2 to 4.The thickness of semi-girder is the 3-30 micron, and the lower floor of this semi-girder (being reflector layer) is metal material, is generally gold, silver or aluminium.Elastic hot occurs when Ear Mucosa Treated by He Ne Laser Irradiation arrives the semi-girder silicon face to expand, thermal expansivity difference due to bi-material, surface micro-structure silicon cantilever generating period photothermal deflection, based on the photothermal deflection principle, the semi-girder that employing has high quality factor (high Q value) picks up the gas absorption light intensity signal, be a kind of picking up signal method with high s/n ratio, neighbourhood noise is had to very strong immunocompetence.
The structural relation of this device is: tunable laser and reflecting object and concave mirror are arranged on same light path, the surface micro-structure silicon cantilever is placed on the focus place of concave mirror, the surface micro-structure silicon face of surface micro-structure silicon cantilever is to concave mirror, the end face of metal surface and optical fiber forms Fa-Po cavity, continuous wave laser is connected by optical fiber with fiber coupler, fiber coupler is connected with optical fiber, between photodetector and fiber coupler, by optical fiber, be connected, the photodetector receiving optical signals also to the electric signal of converting, the output terminal of photodetector is electrically connected to the input end of signal processing system, signal processing system is carried out filtering to electric signal, denoising, data are processed, the output terminal of laser controller is electrically connected to the tunable laser input end, laser instrument is carried out to length scanning and frequency modulation (PFM).
Described optical fiber generally adopts single mode silica fibre or polarization maintaining optical fibre, forms a Fa-Po cavity between the metal surface of its end face and described surface micro-structure silicon cantilever, and its length is generally continuous wave laser and sends 1 ~ 10 times of wavelength.
Described tunable laser generally adopts distributed feedback laser instrument, quantum cascade laser or vertical cavity surface emitting laser etc., its centre wavelength is consistent with the detected gas absorption peak, and can near absorption peak, adjust, for example, when surveying carbon dioxide, can adopt centre wavelength is 1580nm, range of adjustment is ± and the tunable laser of 1nm.
The present invention is as follows with respect to the advantage of prior art:
The first, semi-girder adopts compound surface micro-structure silicon to make, and this structure comprises that to infrared the ultra-wide spectrum zone of visible light part all has very high absorptivity from ultraviolet, therefore can use a device to realize the requirement of wide spectrographic detection; In the situation that do not change system architecture, select the laser instrument of different wave length as exciting light source, do not need to change the concentration detection that the semi-girder sensitive detection parts just can complete multiple or polycomponent trace gas.
Second, the present invention uses surface micro-structure silicon cantilever structure as resonating device, it is a detector that vibration signal is had to the narrow-band filtering function, the surrounding environment optical noise is had to immunocompetence, this will make system antijamming capability under the wide open space environment for use greatly improve, and have that volume is little, cost is low and the characteristics such as portable simultaneously.
The 3rd, this device can be worked under open environment, do not need to adopt photoacoustic cell to reduce ambient noise and system is surveyed to the impact of signal to noise ratio (S/N ratio), therefore be highly suitable for the remote detection to trace gas, particularly the relative traditional optoacoustic spectroscopy detection system of poisonous, the inflammable context of detection with explosive trace gas had to great advantage.
The 4th, adopt the Fabry-perot optical fiber demodulation mode to replace traditional electrolysis to adjust mode, highly sensitive, accuracy of detection is high, and good stability can be eliminated outside electromagnetic interference effectively, has fire-proof and explosion-proof function.
The accompanying drawing explanation
A kind of surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas sniffer of Fig. 1 schematic diagram;
Fig. 2 cantilever beam structure schematic diagram;
Fig. 3 is tunable method amber demodulating system light pick-up schematic diagram;
Fig. 4 surface micro-structure silicon schematic diagram;
The absorption efficiency curve synoptic diagram of Fig. 5 surface micro-structure silicon cantilever.
Embodiment
The photothermal spectroscopy trace gas sniffer based on the surface micro-structure silicon cantilever of working under open environment as shown in Figure 1, tunable laser 1 and reflecting object 2 and concave mirror 4 are on same light path, and surface micro-structure silicon cantilever 3 is placed on the focus place of concave mirror 4.The metal surface 311 of surface micro-structure silicon cantilever 3 forms Fa-Po cavity with the end face of optical fiber 5 51, continuous wave laser 7 is connected by optical fiber 10 with fiber coupler 6, fiber coupler 6 is connected with optical fiber 5, between photodetector 8 and fiber coupler 6, by optical fiber 11, be connected, the photodetector receiving optical signals also to the electric signal of converting.Output terminal at photodetector 8 is electrically connected to the input end of signal processing system 9, and 9 pairs of electric signal of signal processing system carry out filtering, denoising, data processing etc.The output terminal of laser controller 12 is electrically connected to tunable laser 1 input end, and its effect comprises carries out length scanning and frequency modulation (PFM) to laser instrument.
During work, 12 pairs of tunable laser 1 of laser controller are modulated, and modulating frequency is surface micro-structure silicon cantilever 3 natural frequencys
f 0 1/2.By the current scanning mode, laser controller 12 is controlled at place, tested gas absorption peak position to the centre wavelength of tunable laser 1.The light modulated of being sent by tunable laser 1 arrives reflecting object 2 after tested gas.Reflecting object 2 reflexes to the light after gas absorption on concave mirror 4, and concave mirror 4 focuses on it on semi-girder 3.After semi-girder 3 absorbs this energy, resonance occurs.The light sent from light source 7 passes through coupling mechanism 6, then by optical fiber 5, shines on the metal surface 311 of semi-girder, and fiber end face 51 and semi-girder metal surface 311 form the long tuning Fa-Po cavities in a chamber, and wherein fiber end face 51 is fixing.A laser part in optical fiber 5 is reflected back optical fiber 5 by fiber end face 51; Another part is by 311 reflections of semi-girder metal surface, and two bundle reflected light, simultaneously in the interior transmission of optical fiber 5, form interference light.Interference light enters photodetector 8 by fiber coupler 6, and the electric signal that photodetector output is corresponding with interference light intensity also enters signal processing system 9, and 9 pairs of electric signal of signal processing system carry out the data processing, and then calculate tested gas concentration.
As shown in Figure 2, it is double-decker to described semi-girder 3 structures, and upper strata is surface micro-structure silicon 32.Lower floor is the metal material 31 different from surface micro-structure silicon thermal expansivity.Surface micro-structure silicon 32 as shown in Figure 4, this surface micro-structure silicon be adopt pressure at 60Kpa under the sulfur hexafluoride etchant gas environment between 80Kpa, adopt femtosecond laser to etch a plurality of micro-cone structures 321 on the upper surface with silicon on the insulation course of three-decker, erode the middle layer of silicon on insulation course with hydrofluorite, the superiors are taken off, obtain ultrathin bendable surface micro-structure silicon 32, its thickness 2.5-28 micron, plate layer of metal material 31 at the back side of microstructure silicon again, obtain semi-girder 3, gross thickness 3-30 micron.
Light intensity after 3 pairs of tested gas absorption of described semi-girder pick up principle as shown in Figure 3, based on the photothermal deflection principle, vibration as shown in the figure occurs after absorbing the light intensity signal after gas absorption focused on by concave mirror 4 in semi-girder 3, and Oscillation Amplitude is linear with the light intensity signal after gas absorption.Gas concentration is higher, larger by the light intensity of gas absorption, and the light intensity incided on semi-girder 3 is less, and the amplitude of semi-girder 3 is less.Semi-girder metal surface 311 and the Fa-Po cavity that fiber end face 51 forms, surveyed by the interference light intensity to entering optical fiber 5, thereby can be obtained by the light intensity after gas absorption.
As shown in Figure 5, this semi-girder is having very high absorption efficiency to the absorption efficiency curve of described surface micro-structure silicon cantilever from the ultraviolet to the region of ultra-red, and the absorption efficiency curve is more smooth.
Claims (10)
1. a surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas detection method, it is characterized in that, described method is to allow the pulse laser sent from tunable laser pass through detected gas, after being absorbed, pulse laser incides on reflecting object, process reflecting object back reflection is to concave mirror, with concave mirror, the luminous energy received is focused on the surface micro-structure silicon cantilever, after absorbing luminous energy by the surface micro-structure silicon cantilever, resonance occurs, the tunable Fabry-perot optical fiber demodulating system simultaneously formed by the metal surface based on fiber end face and semi-girder is picked up the vibration signal of this surface micro-structure silicon cantilever, when semi-girder generation resonance, the chamber length of Fa-Po cavity changes, thereby cause the variation of reflection interference light intensity generating period, obtain the resonance signal of semi-girder by the intensity demodulation to this light signal, finally adopt signal processing system to be finally inversed by the concentration that is detected gas,
Described surface micro-structure silicon cantilever (3) is double-decker, upper strata is surface micro-structure silicon, lower floor is metal, elastic hot occurs when pulsed laser irradiation arrives the semi-girder silicon face to expand, due to the thermal expansivity difference of two layers of material, surface micro-structure silicon cantilever generating period photothermal deflection;
The modulating frequency of described tunable laser (1) is 1/2 of surface micro-structure silicon cantilever resonance frequency, and its centre wavelength is consistent with the detected gas absorption peak;
The chamber of described Fa-Po cavity is long sends 1 ~ 10 times of wavelength for continuous wave laser.
2. surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas detection method according to claim 1, it is characterized in that, described surface micro-structure silicon cantilever (3) thickness is the 3-30 micron, the surface micro-structure silicon on its upper strata comprises a plurality of micro-cone structures, and the thickness of micro-cone structure is the 2.5-28 micron;
The upper strata of described surface micro-structure silicon cantilever is to obtain by the following method: gas pressure intensity at 60Kpa in the sulfur hexafluoride gas environment between 80Kpa, the upper surface of silicon on insulation course, etch a plurality of micro-cone structures with femtosecond laser, then erode the middle layer of silicon on insulation course with hydrofluorite, finally uppermost surface is stripped down, obtain ultra-thin surface micro-structure silicon.
3. a surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas sniffer of realizing claim 1 or 2 described method, it is characterized in that, comprise tunable laser (1), reflecting object (2), surface micro-structure silicon cantilever (3), concave mirror (4), the first optical fiber (5), fiber coupler (6), continuous wave laser (7), photodetector (8), signal processing system (9), the second optical fiber (10), the 3rd optical fiber (11) and laser controller (12);
Described surface micro-structure silicon cantilever (3) is double-decker, upper strata is surface micro-structure silicon, and lower floor is metal, elastic hot occurs when Ear Mucosa Treated by He Ne Laser Irradiation arrives the semi-girder silicon face and expand, due to the thermal expansivity difference of two layers of material, surface micro-structure silicon cantilever generating period photothermal deflection;
Described tunable laser (1) is arranged on same light path with reflecting object (2) and concave mirror (4), surface micro-structure silicon cantilever (3) is placed on the focus place of concave mirror (4), the surface micro-structure silicon face of surface micro-structure silicon cantilever (3) is to concave mirror (4), metal surface (311) forms Fa-Po cavity with the end face (51) of the first optical fiber (5), continuous wave laser (7) is connected by the second optical fiber (10) with fiber coupler (6), fiber coupler (6) is connected with the first optical fiber (5), between photodetector (8) and fiber coupler (6), by the 3rd optical fiber (11), be connected, the photodetector receiving optical signals also to the electric signal of converting, the output terminal of photodetector (8) is electrically connected to the input end of signal processing system (9), signal processing system (9) is carried out filtering to electric signal, denoising, data are processed, the output terminal of laser controller (12) is electrically connected to tunable laser (1) input end, laser instrument is carried out to length scanning and pulse frequency modulation,
The modulating frequency of described tunable laser (1) is 1/2 of surface micro-structure silicon cantilever resonance frequency, and its centre wavelength is consistent with the detected gas absorption peak;
The chamber of described Fa-Po cavity is long sends 1 ~ 10 times of wavelength for continuous wave laser.
4. surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas sniffer according to claim 3, it is characterized in that, described surface micro-structure silicon cantilever (3) thickness is the 3-30 micron, upper surface microstructure silicon comprises a plurality of micro-cone structures, and the thickness of micro-cone structure is the 2.5-28 micron.
5. surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas sniffer according to claim 3, is characterized in that, described micro-cone structure is micron and nano-scale, is pyramid, and the ratio of cone height and bottom surface diameter is between 2 to 4.
6. surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas sniffer according to claim 3, it is characterized in that, described upper surface microstructure silicon is to obtain by the following method: gas pressure intensity at 60Kpa in the sulfur hexafluoride gas environment between 80Kpa, the upper surface of silicon on insulation course, etch a plurality of micro-cone structures with femtosecond laser, then erode the middle layer of silicon on insulation course with hydrofluorite, finally uppermost surface is stripped down, obtain ultra-thin surface micro-structure silicon.
7. surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas sniffer according to claim 3, is characterized in that, described tunable laser adopts distributed feedback laser instrument, quantum cascade laser or vertical cavity surface emitting laser.
8. surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas sniffer according to claim 3, is characterized in that, described photodetector is the single-point photodetector.
9. surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas sniffer according to claim 3, it is characterized in that, described the first optical fiber adopts single mode silica fibre or polarization maintaining optical fibre, forms a Fa-Po cavity between the metal surface of the end face of the first optical fiber and described surface micro-structure silicon cantilever.
10. surface microstructure silicon cantilever enhancement type optical-thermal spectrum trace gas sniffer according to claim 3, is characterized in that, the metal material of semi-girder lower floor is gold, silver or aluminium.
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| CN103884419B (en) * | 2014-04-17 | 2017-01-11 | 山西大学 | Tuning fork type quartz crystal oscillator resonant frequency measurement method based on optical excitation and device |
| CN104655587A (en) * | 2015-02-14 | 2015-05-27 | 合肥知常光电科技有限公司 | Extra-high sensitive gas absorption spectrum measuring system and method based on MEMS |
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