CN106054300B - A kind of CO2Gas detection binary channels infrared fileter and preparation method thereof - Google Patents

A kind of CO2Gas detection binary channels infrared fileter and preparation method thereof Download PDF

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CN106054300B
CN106054300B CN201610592825.6A CN201610592825A CN106054300B CN 106054300 B CN106054300 B CN 106054300B CN 201610592825 A CN201610592825 A CN 201610592825A CN 106054300 B CN106054300 B CN 106054300B
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binary channels
film
air
infrared fileter
sub
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CN106054300A (en
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乔冠军
侯海港
邵海成
刘桂武
王明松
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Weijidian Technology (Suzhou) Co.,Ltd.
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Jiangsu University
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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00Optical elements other than lenses
    • G02B5/20Filters
    • G02B5/28Interference filters
    • G02B5/281Interference filters designed for the infrared light
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00Optical elements other than lenses
    • G02B5/20Filters
    • G02B5/28Interference filters
    • G02B5/285Interference filters comprising deposited thin solid films
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N2021/3595Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR

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  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
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  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The present invention relates to infrared fileters, and in particular to a kind of CO2Gas detection binary channels infrared fileter and preparation method thereof.Base material selects single crystalline Si, refractive index n=3.42881;High-index material selects Ge, refractive index n=4.16422;Low-index material selects SiO, refractive index n=1.81312;Deposit the membrane system of different centre wavelengths respectively on two surfaces of substrate.4260nm and 2780nm binary channels infrared fileter provided by the invention, two peak transmittances up to more than 90%, greatly improve signal-to-noise ratio, inhibit the interference of other gases well, improve instrument detection accuracy and efficiency.

Description

A kind of CO2Gas detection binary channels infrared fileter and preparation method thereof
Technical field
The present invention relates to infrared fileters, and in particular to a kind of CO2Gas detection binary channels infrared fileter and its system Preparation Method.
Background technology
It is required in metallurgy, aerospace, agricultural, medical treatment, environmental protection etc. to CO2Concentration carry out quantitative detection and control System, and application environment is very severe in many cases, such as inflammable and explosive, high temperature, high pressure, has magnetic field occasion.Therefore, it develops Stability is good, selectivity is good, high sensitivity, miniaturized and portable CO2Gas sensor has very high practical value.
Infrared spectrum analyser is the instrument that gas content is measured using gas infrared signature absorption peak, selects the red of specific wavelength Outer gas analysis filter is the critical component of infrared gas analyser.The light that light source is sent out obtains certain after optical filter The quasi-monochromatic light (the narrower degree of monochromaticity of bandwidth is better) of bandwidth, after which is actually taken up by gas by gas sample cell, is examined by detector Survey output intensity.Due to CO2Gas has stronger characteristic absorption spectrum in certain wave strong point, by probe gas to specific wavelength The attenuation of infrared spectrum can calculate its CO2Content.
According to data-searching, such as document " research of woods Zhe .TPS2534 new infrared gas concentration sensors and application electricity Big science and engineering, 2011,246 (1):10-12. " TPS2534 new infrared gas concentration sensors are more and more to be applied to infrared-gas In the production and design of Concentration Testing instrument.For CO2Gas concentration detects, main to select TPS2534G2 models optical filter peace Mounted in the sensing window of TPS2534 sensors, centre wavelength is 4.26 μm, centre wavelength deviation ± 1%, halfwidth for 180 ± 20nm, halfwidth/centre wavelength are 4.2%, and peak transmission is more than 73%." 4.26 microns of Chinese patent ZL95244862.9 For spike filter " using white stone as substrate, ZnSe and ZnTi are high low-index material, design central wavelength lambda 0=4.26 ± 0.01 μm, halfwidth λ 0.50=0.14 ± 0.02 μm, 0.10/ Δ λ 0.00≤1.4 of form factor η=Δ λ, peak transmission The 4260nm spike filters of Tmax >=70%.
But the equal single bandpass optical filter of above two optical filter, and passband is wider, cut-off wave band is not wide enough, peak transmission It is relatively low, so measurement accuracy, stability and jamproof ability are also to be hoisted, poor sensitivity, it is impossible to meet market hair The needs of exhibition.
Invention content
A kind of binary channels and peak transmittance are provided the purpose of the present invention is to solve above-mentioned the deficiencies in the prior art Height can greatly improve signal-to-noise ratio, effectively detect CO2Binary channels band logical infrared fileter of gas and preparation method thereof.
To achieve these goals, a kind of CO designed by the present invention2Gas detection with binary channels infrared fileter and its Preparation method, it is characterized in that:
(1) substrate, silicon twin polishing, 300 ± 10 μm of thickness, crystal orientation are made using single crystalline Si<100>.
(2) Coating Materials selection silicon monoxide SiO and monocrystalline germanium Ge, multi-coated interference is deposited on two surfaces of substrate respectively Film.
(3) wherein a face film structure uses: Air/ 0.54L0.39H1.1L0.64H1.45L5.61H1.5L0.27H1.1L1.17H0.97L3.99H0.97L1.22H0.517L1.89 H1.128L5.91HL1.4H1.48L1.9H1.43L1.38H0.04L1.27H1.51L1.524H1.175L0.2H1.32L1.352 H1 .53L1.34H1.28L/Sub, central wavelength lambda1=4260nm.
(4) another side film structure uses: Air/ 1.6L1.44H0.34L4.32H0.88L0.92H0.95L0.99H1.03L0.22H0.11L1.728H0.96L0.97H0.87L1. 06H2.53L6.16H1.38L0.65H0.41L/Sub, central wavelength lambda2=2780nm.
Symbol meaning is respectively in membrane system:Sub is substrate, and Air is air, and H and L represent film layer Ge (high refractive indexes respectively Material layer) and film layer SiO (low refractive index material layer) 1/4 wave optical thickness, centre wavelength is respectively λ1= 4260nm, λ2=2780nm, 1H=(4nHd)/λ;1L=(4nLD)/λ, number is the thickness coefficient of film layer in structural formula.
A kind of above-mentioned CO2Gas detection binary channels infrared fileter and preparation method thereof, using crystal silicon Si as substrate, one Silicon oxide sio and germanium Ge are Coating Materials, prepare film plating layer using the method for vacuum thermal evaporation thin film deposition, Ge selects electronics Beam is deposited, deposition rate 8SiO selects porous molybdenum boat resistance heating vapor deposition, deposition rate 40Start to steam It is 1.0 × 10 to plate vacuum degree-3Pa, depositing temperature are 200 DEG C.
A kind of above-mentioned CO2Gas detection binary channels infrared fileter and preparation method thereof, using optical monitor control Layer thickness is film-made, and is aided with quartz-crystal control control deposition rate.
A kind of above-mentioned CO2Gas detection binary channels infrared fileter and its 4260nm and 2780nm being prepared Dual band pass infrared fileter;Air/ of the centre wavelength for 4260nm is used on one side 0.54L0.39H1.1L0.64H1.45L5.61H1.5L0.27H1.1L1.17H0.97L3.99H0.97L1.22H0.517L 1.89H1.128L5.91HL1.4H1.48L1.9H1.43L1.38H0.04L1.27H1.51L1.524H1.175L0.2H1.32 L1.352H1.53L1.34H1.28L/Sub film structures realize that 2750nm~2800nm and 4150nm~4350nm wave bands are high Transmission, and in addition to the passband of centre wavelength 2780nm bandwidth 75nm, all cut from remaining spectrum in the range of 2000~3500nm Only;Another side uses Air/ of the centre wavelength for 2780nm 1.6L1.44H0.34L4.32H0.88L0.92H0.95L0.99H1.03L0.22H0.11L1.728H0.96L0.97H0.8 7L1.06H2.53L6.16H1.38L0.65H0.41L/Sub film structure, realization 4200nm~4300nm and 2700nm~ 2840nm wave bands are highly transmissive, and in addition to the passband of centre wavelength 4260nm bandwidth 140nm, in the range of 3500~8500nm Remaining spectrum all ends;Two sides coordinates, final to realize, 4240nm~4280nm and 2750nm~2800nm wave bands are average saturating Rate is crossed not less than 92%, halfwidth is respectively 145nm and 75nm, except centre wavelength 4260nm and 2780nm bandwidth 140nm and Outside the passband of 75nm, all end from remaining spectrum in the range of 2000~8500nm, 2000nm~2700nm average transmittances It is that 0.112%, 4400nm~8500nm average transmittances are for 0.089%, 2840nm~4100nm average transmittances 0.019%, signal-to-noise ratio can be greatly improved, can be very good to inhibit the interference of other gases, product optical property and physics are strong Degree is well positioned to meet actual operation requirements, is widely used in CO2Gas infrared acquisition instrument improves instrument detection accuracy and effect Can, can accomplish more rapidly, more accurately confirm leakage point.
Compared with the prior art, the present invention has the following advantages:
1st, Double-channel optical filter and tradition CO2Detection is compared with optical filter, and tool is CO there are two transmission narrowband2's Characteristic absorption wave band can effectively improve the measurement sensitivity and precision of instrument.
2nd, for Double-channel optical filter compared with traditional technology method, the narrowband that there is centre wavelength to be 4260nm and 2780nm is saturating Spectrum is crossed, the rising edge and failing edge of transmission bands are precipitous, and waveform rectangular degree is good, peak transmittance>90%th, end in cut-off region Depth<0.1%, therefore the transmission that effective service band of 4260nm and 2780nm can be as big as possible, and remaining invalid wave band Background noise then greatly reduce, thus excellent signal-to-noise ratio can be obtained, improve the measurement sensitivity and precision of instrument.
3rd, the filter technology that prepared by the present invention is simple, can form batch production, and performance is stablized, and meets high-precision CO2 The performance requirement of gas infrared acquisition instrument.
Description of the drawings
Fig. 1 is CO of the present invention2The structure diagram of gas detection binary channels infrared fileter;
Wherein:Substrate 1 is single crystalline Si, and film material 2 is Ge, and film material 3 is SiO.
Fig. 2 is Double-channel optical filter final performance measured curve figure.
Specific embodiment
The present invention is further described with reference to the accompanying drawings and examples.
Embodiment 1:
As shown in Figure 1, a kind of CO provided in this embodiment2Gas detection binary channels infrared fileter and preparation method thereof It is:
(1) size is used to make substrate, silicon twin polishing, 300 ± 10 μm of thickness, crystal orientation for the single crystalline Si of Φ 50.8<100>.
(2) Coating Materials selection silicon monoxide SiO and monocrystalline germanium Ge, multi-coated interference is deposited on two surfaces of substrate respectively Film.
(3) wherein a face film structure uses: Air/0.54L0.39H1.1L0.64H1.45L5.61H1.5L0.27H1. 1L1.17H0.97L3.99H0.97L1.22H0.517L1.89 H1.128L5.91HL1.4H1.48L1.9H1.43L1.38H0. 04L1.27H1.51L1.524H1.175L0.2H1.32L1.352H1 .53L1.34H1.28L/Sub, central wavelength lambda1= 4260nm。
(4) another side film structure uses: Air/1.6L1.44H0.34L4.32H0.88L0.92H0.95L0.99H1. 03L0.22H0.11L1.728H0.96L0.97H0.87L1. 06H2.53L6.16H1.38L0.65H0.41L/Sub, middle cardiac wave Long λ2=2780nm.
Symbol meaning is respectively in membrane system:Sub is substrate, and Air is air, and H and L represent film layer Ge (high refractive indexes respectively Material layer) and film layer SiO (low refractive index material layer) 1/4 wave optical thickness, centre wavelength is respectively λ1= 4260nm, λ2=2780nm, 1H=(4nHd)/λ;1L=(4nLD)/λ, number is the thickness coefficient of film layer in structural formula.
A kind of CO provided in this embodiment2Gas detection binary channels infrared fileter and preparation method thereof, with monocrystalline silicon Si is substrate, and silicon monoxide SiO and germanium Ge are Coating Materials, and film plating layer is prepared using the method for vacuum thermal evaporation thin film deposition, Ge selects electron beam evaporation plating, deposition rate 8SiO selects porous molybdenum boat resistance heating vapor deposition, deposition rate 40It is 1.0 × 10 to start that vacuum degree is deposited-3Pa, depositing temperature are 200 DEG C.
Due to specifically how to evaporate using electron gun evaporation and being those skilled in the art using resistance heating evaporation plated film The routine techniques grasped, no further details to be given herein.
A kind of Double-channel optical filter provided in this embodiment uses is coated with Air/0.54L0.39H1.1L0.64H1. on one side 45L5.61H1.5L0.27H1.1L1.17H0.97L3.99H0.97L1.22H0.517L 1.89H1.128L5.91HL1.4H1. 48L1.9H1.43L1.38H0.04L1.27H1.51L1.524H1.175L0.2H1.32 L1.352H1.53L1.34H1.28L/ Sub membrane systems realize that 4200nm~4300nm and 2700nm~2840nm wave bands are highly transmissive, and except centre wavelength 4260nm bandwidth Outside the passband of 140nm, all end from remaining spectrum in the range of 3500~8500nm;Another side Air/ 1.6L1.44H0.34L4.32H0.88L0.92H0.95L0.99H1.03L0.22H0.11L1.728H0.96L0. 97H0.8 7L1.06H2.53L6.16H1.38L0.65H0.41L/Sub membrane systems, realization 2750nm~2800nm and 4150nm~ 4350nm wave bands are highly transmissive, and in addition to the passband of centre wavelength 2780nm bandwidth 75nm, from its in the range of 2000~3500nm The all cut-offs of remaining light spectrum.
CO provided in this embodiment2Gas detection binary channels infrared fileter, the centre wavelength of two narrowband position Precision controls thicknesses of layers within 0.4%, to membrane system using optical monitor, and is aided with quartz-crystal control control deposition speed Rate.
Prepared optical filter is surveyed using German 70 type Fourier infrared spectrographs of Bruker companies VERTEX Examination.The optical filter final performance measured curve figure of this optical filter final performance structure such as Fig. 2:
1. central wavelength lambda1=4260nm, λ2=2780nm;
2. bandwidth Delta lambda1=140nm, Δ λ2=75nm;
3. form factor Δ λ1 (10%)/Δλ1 (50%)=1.28, Δ λ2 (10%)/Δλ2 (50%)=1.33;
4. peak transmittance Tp1=92.92%, Tp2=92.84%;
5. 2000~8500nm T in addition to passbandavg≤ 0.1%.
The above is only presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, every according to the present invention Any simple modification, change and the equivalent structure transformation that technical spirit makees above example, still fall within skill of the present invention In the protection domain of art scheme.

Claims (4)

1. a kind of CO2Gas detection binary channels infrared fileter, it is characterised in that:
(1) substrate, silicon twin polishing, 300 ± 10 μm of thickness, crystal orientation are made using single crystalline Si<100>;
(2) Coating Materials selects silicon monoxide SiO and monocrystalline germanium Ge, and it is thin to deposit multi-coated interference respectively on two surfaces of substrate Film;
(3) wherein a face film structure uses:Air/0.54L0.39H1.1L0.64H1.45L5.61H1.5L0.27H1.1L1. 17H0.97L3.99H0.97L1.22H0.517L1.89H1.128L5.91HL1.4H1.48L1.9H1.43L1.38H0.04L1.2 7H1.51L1.524H1.175L0.2H1.32L1.352H1.53L1.34H1.28L/Sub, central wavelength lambda1=4260nm;
(4) another side film structure uses:Air/1.6L1.44H0.34L4.32H0.88L0.92H0.95L0.99H1.03L0. 22H0.11L1.728H0.96L0.97H0.87L1.06H2.53L6.16H1.38L0.65H0. 41L/Sub, central wavelength lambda2= 2780nm;
Symbol meaning is respectively in membrane system:Sub is substrate, and Air is air, H and L represent respectively high-index material film layer Ge and 1/4 wave optical thickness of low-index material film layer SiO, centre wavelength is respectively λ1=4260nm, λ2=2780nm, 1H=(4nHd)/λ;1L=(4nLD)/λ, number is the thickness coefficient of film layer in structural formula.
2. a kind of CO as described in claim 12Gas detection binary channels infrared fileter, it is characterised in that:Using Vacuum Heat The method of thin evaporated film deposition prepares film plating layer, and Ge selects electron beam evaporation plating, and deposition rate isSiO selects porous molybdenum Boat resistance heating is deposited, and deposition rate isIt is 1.0 × 10 to start that vacuum degree is deposited-3Pa, depositing temperature are 200 DEG C.
3. a kind of CO as claimed in claim 22Gas detection binary channels infrared fileter, it is characterised in that:It is supervised using optics Control method controls thicknesses of layers, and is aided with quartz-crystal control control deposition rate.
4. a kind of CO as described in claim 12Gas detection binary channels infrared fileter, it is characterised in that:In using on one side The Air/0.54L0.39H1.1L0.64H1.45L5.61H1.5L0.27H1.1L1.17H0.97L 3. of a length of 4260nm of cardiac wave 99H0.97L1.22H0.517L1.89H1.128L5.91HL1.4H1.48L1.9H1.43L1.38H0.04L1.27H1.51L1.5 24H1.175L0.2H1.32L1.352H1.53L1.34H1.28L/Sub film structures, realize 2750nm~2800nm and 4150nm~4350nm wave bands are highly transmissive, and in addition to the passband of centre wavelength 2780nm bandwidth 75nm, from 2000~3500nm models Remaining spectrum in enclosing all ends;Another side uses Air/ of the centre wavelength for 2780nm 1.6L1.44H0.34L4.32H0.88L0.92H0.95L0.99H1.03L0.22H0.11L1.728H0.96L0.97H0.87L1. 06H2.53L6.16H1.38L0.65H0.41L/Sub film structures realize 4200nm~4300nm and 2700nm~2840nm waves Section is highly transmissive, and in addition to the passband of centre wavelength 4260nm bandwidth 140nm, complete from remaining spectrum in the range of 3500~8500nm End in portion;Two sides coordinates, and final to realize, 4240nm~4280nm and 2750nm~2800nm wave band mean transmissivities are not less than 92%, halfwidth is respectively 145nm and 75nm, in addition to the passband of centre wavelength 4260nm and 2780nm bandwidth 140nm and 75nm, All to end from remaining spectrum in the range of 2000~8500nm, 2000nm~2700nm average transmittances are 0.089%, 2840nm~4100nm average transmittances are that 0.112%, 4400nm~8500nm average transmittances are 0.019%, can be greatly Improve signal-to-noise ratio.
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CN106990466B (en) * 2017-04-24 2020-01-24 江苏大学 Narrow-band optical filter and preparation method thereof
CN108801967B (en) * 2018-06-21 2021-06-15 长春理工大学 Double-passband filter device, infrared thermal imaging detection system and method for detecting methane
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CN103713349A (en) * 2013-11-29 2014-04-09 杭州麦乐克电子科技有限公司 Medical infrared gas detection and analysis filter with central wavelength of 6557 nm
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