CN105842770B - A kind of CO2Gas detection infrared fileter and preparation method thereof - Google Patents
A kind of CO2Gas detection infrared fileter and preparation method thereof Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000012528 membrane Substances 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 238000004062 sedimentation Methods 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 238000007747 plating Methods 0.000 claims abstract description 7
- 238000002834 transmittance Methods 0.000 claims abstract description 7
- 229910021419 crystalline silicon Inorganic materials 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims abstract description 5
- 238000007740 vapor deposition Methods 0.000 claims abstract description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000005485 electric heating Methods 0.000 claims abstract description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 4
- 239000011733 molybdenum Substances 0.000 claims abstract description 4
- 238000005566 electron beam evaporation Methods 0.000 claims abstract description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 31
- 230000003287 optical effect Effects 0.000 claims description 19
- 239000011248 coating agent Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 229910052732 germanium Inorganic materials 0.000 claims description 4
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000001228 spectrum Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 26
- 239000010408 film Substances 0.000 description 25
- 229910002092 carbon dioxide Inorganic materials 0.000 description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 238000002560 therapeutic procedure Methods 0.000 description 2
- 238000000427 thin-film deposition Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/28—Interference filters
- G02B5/281—Interference filters designed for the infrared light
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a kind of CO2Gas detection infrared fileter and preparation method thereof, infrared fileter base material select single crystalline Si, and high-index material selects Ge, and low-index material selects SiO.Deposit main membrane system face film and interference cut-off membrane system face film respectively on two surfaces of substrate, coating process condition is：Wherein Ge selects electron beam evaporation plating, and sedimentation rate isSiO selects porous molybdenum boat electric heating vapor deposition, and sedimentation rate isIt is 1.0 × 10 to start that vacuum degree is deposited‑3Pa, depositing temperature are 200 DEG C.Obtained 4260nm band logical infrared fileters, peak transmittance greatly improve signal-to-noise ratio, inhibit the interference of other gases well, improve instrument detection accuracy and efficiency up to more than 90%.
Description
Technical field
The present invention relates to infrared fileter preparing technical fields, and in particular to a kind of CO2Gas detection infrared fileter
And preparation method thereof.
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, develop
Stability is good, selectivity is good, high sensitivity, the CO of Miniaturized portable2Gas 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 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 at 4260nm wavelength, by probe gas to 4260nm
The attenuation of IR wavelengths 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 narrow band pass 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 narrow band pass filters of Tmax >=70%.
But above two optical filter passband is wider, and cut-off wave band is not wide enough, and peak transmission is relatively low, so measurement is accurate
Property, stability and jamproof ability are also to be hoisted.
Document " such as Zhu Huaxin, Wang Tongtong, high sturdy pines ultra-wide cut-off sideband optical filter research artificial lens journals, 2013,
43(12):Then 2701-2706 " is added by being superimposed the multilayer cycle films of different centre wavelengths between variant cycle film layer
Add transition zone, direct broadening rejection zone width realizes the cut-off depth of 0.5 ﹣, 0.85 μm of cut-off region up to 5 × 10-3Hereinafter, 0.9 ﹣
Mean transmissivity in 1.3 μm of passbands also reaches 83.14% ultra-wide cut-off sideband optical filter research.But it is secondary to eliminate transmission
Peak adds more transition zone, makes the coating single side number of plies up to 57 layers, and rejection zone width is only 0.35 μm, and cut-off depth is also paid no attention to
Think.Document " Li Dongmei, Liu Shuan pay the research photon journals of broadband bandpass filter in the infrared therapy apparatus such as elegant China,
2015,44 (3):0301001 " uses the design philosophy of " splitting technology requirement ", and the overall technology requirement of optical filter is carried out carefully
Change and split, new membrane system is designed by the requirement after fractionation, and double coated is carried out in K9 substrate of glass, pass through two-sided superposition
Mode finally realizes that 600 ﹣ 1200nm wave bands mean transmissivities are more than 95%, and 300~550nm, 1270~2000nm wave bands are averaged
Transmitance is less than 1%, broadband bandpass filter in infrared therapy apparatus.But its split after be all using a kind of basic membrane system into
Row design and optimization, causing two face mask layer numbers, preparation process difficulty is larger and changes using cut-off type glass as substrate up to 173 layers
Method.Document " Li Dongmei, Wang Xiaojuan pay the development photon journals of the wide cut-off narrow band pass filter of the near-infrareds such as elegant China,
2014,43 (1):0131002 " uses conventional multicavity Film System of Narrow band by front, and reverse side uses interference stopping lightscreening plate
Membrane system finally realizes 1530~1600nm wave bands mean transmissivity higher than 92%, 800~1530nm, 1600~1800nm wave bands
The development of mean transmissivity cut-off narrow band pass filter wide less than 0.3% near-infrared.But front membrane material using TiO2 and
SiO2, reverse side uses Si and SiO2, although being effectively reduced reverse side film layer, also increases and prepares difficulty and cut-off wave band
It is relatively narrow, while up to 33 layers of front conventional multicavity Film System of Narrow band, it needs further to optimize.
But just currently used for measure carbon dioxide 4260nm band logical infrared fileters, passband is wider, end wave band
Not wide enough, peak transmission is relatively low, so measurement accuracy, stability and jamproof ability are also to be hoisted, sensitivity
Difference, it is impossible to meet the needs of market development.
The content of the invention
It is high that a kind of peak transmittance is provided the purpose of the present invention is to solve above-mentioned the deficiencies in the prior art, it can be greatly
Raising signal-to-noise ratio, effectively detect CO24260nm band logical infrared fileters of gas and preparation method thereof.
To achieve these goals, a kind of CO designed by the present invention2Gas detection infrared fileter, it is characterized in that：
(1) substrate is made using single crystalline Si；Silicon twin polishing, 300 ± 10 μm of thickness, crystal orientation<100>.
(2) Coating Materials selection silicon monoxide SiO and monocrystalline germanium Ge, main membrane system face is deposited on two surfaces of substrate respectively
Film and interference cut-off membrane system face film.
(3) main membrane system face membrane structure uses Air/1.16L1.232HL 6HLHLHL 4HLHLHL 6HLH/Sub.
(4) interference cut-off membrane system face film uses：Sub/0.42(HL)9 0.65(HL)8 1.53(HL)6/Air。
Symbol meaning is respectively in membrane system：Sub is substrate, and Air is air, and H and L represent film layer Ge (highs index of refraction respectively
Material layer) and film layer SiO (low refractive index material layer) 1/4 wave optical thickness, central wavelength lambda=4260nm, 1H=
(4nHd)/λ；1L=(4nLD)/λ, number is the thickness coefficient of film layer in structural formula, the index in structural formula is membrane stack plated film
Periodicity.
A kind of above-mentioned CO2The preparation method of gas detection infrared fileter, using crystal silicon Si as substrate, silicon monoxide
SiO and germanium Ge is Coating Materials, and film plating layer is prepared using the method for vacuum thermal evaporation thin film deposition, and Ge selects electron beam evaporation plating,
Sedimentation rate is/sec；SiO selects porous molybdenum boat electric heating vapor deposition, and sedimentation rate is/ sec, starting vapor deposition vacuum degree is
1.0×10-3Pa, depositing temperature are 200 DEG C.
A kind of above-mentioned CO2The preparation method of gas detection infrared fileter is thick using optical monitor control film layer
Degree, and it is aided with quartz-crystal control control sedimentation rate.
The above-mentioned 4260nm band logical infrared fileters being prepared, main membrane system use multi-cavity narrowband film structure, cooperation
The interference cut-off membrane system of height cut-off depth, centre wavelength 4260nm, 4240nm~4280nm wave band mean transmissivity are
91.83%, halfwidth 100nm；In addition to the passband of centre wavelength 4260nm bandwidth 100nm, from 1500~10000nm scopes
Remaining interior spectrum all ends, and 1500nm~4180nm average transmittances are average saturating for 0.038%, 4350nm~8000nm
Rate is penetrated as 0.044%, can greatly improve signal-to-noise ratio, can be very good to inhibit the interference of other gases, product optical property and
Physical strength is well positioned to meet actual operation requirements, is widely used in CO2Gas infrared acquisition instrument improves instrument detection essence
Degree and efficiency, can accomplish more rapidly, more accurately confirm leakage point.
The present invention has the following advantages compared with prior art：
1st, optical filter has the narrowband that centre wavelength is 4260nm through spectrum, transmission bands compared with traditional technology method
Rising edge and trailing edge it is precipitous, waveform rectangular degree is good, peak transmittance>90%th, cut-off depth in cut-off region<0.1%, because
Effective service band of this 4260nm can be as big as possible transmission, and the background noise of remaining invalid wave band is then great
Reduce, thus excellent signal-to-noise ratio can be obtained, improve the measurement sensitivity and precision of instrument.
2nd, 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 infrared fileter；
Wherein：Substrate 1 is single crystalline Si, and film material 2 is Ge, and film material 3 is SiO.
Fig. 2 is optical filter final performance measured curve figure.
Specific embodiment
Embodiment 1
The present invention is further described with reference to the accompanying drawings and examples.
Embodiment 1：
As shown in Figure 1, a kind of CO2 gases detection infrared fileter provided in this embodiment and preparation method thereof is：
(1) size is used to make substrate for the single crystalline Si of Φ 50.8；Silicon twin polishing, 300 ± 10 μm of thickness, crystal orientation<100
>。
(2) Coating Materials selection SiO and monocrystalline Ge on two surfaces of substrate deposits main membrane system face film A and does respectively
Relate to cut-off membrane system face film B.
(3) main membrane system face membrane structure uses Air/1.16L1.232HL 6HLHLHL 4HLHLHL 6HLH/Sub.
(4) interference cut-off membrane system face film uses：Sub/0.42(HL)9 0.65(HL)8 1.53(HL)6/Air。
Symbol meaning is respectively in membrane system：Sub is substrate, and Air is air, and H and L represent film layer 2 (Ge) (height folding respectively
Penetrate rate material layer) and film layer 3 (SiO) (low refractive index material layer) 1/4 wave optical thickness, central wavelength lambda=
4260nm, 1H=(4nHd)/λ；1L=(4nLD)/λ, in structural formula number be the thickness coefficient of film layer, the index in structural formula
It is the periodicity of membrane stack plated film.
A kind of preparation method of CO2 gases detection infrared fileter provided in this embodiment, using monocrystalline silicon Si as substrate,
Silicon monoxide SiO and germanium Ge is Coating Materials, prepares film plating layer using the method for vacuum thermal evaporation thin film deposition, Ge selects electricity
Beamlet is deposited, and sedimentation rate is/sec.SiO selects porous molybdenum boat electric heating vapor deposition, and sedimentation rate is/ sec starts to steam
It is 1.0 × 10 to plate vacuum degree-3Pa, depositing temperature are 200 DEG C.
By specifically how to evaporate using electron gun evaporation and being those skilled in the art institute using resistance steaming evaporation coating
The routine techniques of grasp, no further details to be given herein.
A kind of optical filter provided in this embodiment plates multi-cavity narrowband membrane system using one side, improves the transmission of effective service band
Rate and waveform rectangular degree, once improve valid signal strengths；The interference cut-off membrane system of the high cut-off depth of another side plating, reaches 1500
All invalid secondary peaks in the range of~8000nm in addition to passband.
CO provided in this embodiment2Gas detection infrared fileter, centre wavelength positioning accuracy within 0.4%,
Thicknesses of layers is controlled using optical monitor to membrane system, and is aided with quartz-crystal control control sedimentation 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 lambda=4260nm；
2. bandwidth Delta lambda=100nm；
3. form factor Δ λ 10%/Δ λ 50%=1.47；
4. peak transmittance Tp=91.83%；
1500~8000nm T in addition to passbandavg≤ 0.05%.
The above is only presently preferred embodiments of the present invention, not the present invention imposed any restrictions, it is 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 infrared fileter, it is characterised in that：
(1) substrate is made using single crystalline Si；Silicon twin polishing, 300 ± 10 μm of thickness, crystal orientation<100>；
(2) Coating Materials selection silicon monoxide SiO and monocrystalline germanium Ge, main membrane system face film is deposited on two surfaces of substrate respectively
With interference cut-off membrane system face film；
(3) main membrane system face membrane structure uses Air/1.16L1.232HL 6HLHLHL 4HLHLHL 6HLH/Sub；
(4) interference cut-off membrane system face film uses：Sub/0.42(HL)9 0.65(HL)8 1.53(HL)6/Air；
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, central wavelength lambda=4260nm, 1H=(4nHd)/λ；1L=
(4nLD)/λ, number is the thickness coefficient of film layer in structural formula, the index in structural formula is the periodicity of membrane stack plated film.
2. a kind of CO as described in claim 12Gas detection infrared fileter, it is characterised in that：It is thin using vacuum thermal evaporation
The method of film deposition prepares film plating layer, and Ge selects electron beam evaporation plating, and sedimentation rate isSiO selects porous molybdenum boat electric heating
Vapor deposition, sedimentation rate areIt 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 infrared fileter, it is characterised in that：Using optical monitor control
Layer thickness is film-made, and is aided with quartz-crystal control control sedimentation rate.
4. a kind of CO as described in claim 12Gas detection infrared fileter, it is characterised in that：The infrared fileter,
Main membrane system uses multi-cavity narrowband film structure, coordinates the interference cut-off membrane system of high cut-off depth, centre wavelength 4260nm,
4240nm~4280nm wave bands mean transmissivity is 91.83%, halfwidth 100nm；Except centre wavelength 4260nm bandwidth 100nm
Passband outside, all end from remaining spectrum in the range of 1500~10000nm, 1500nm~4180nm average transmittances are
0.038%, 4350nm~8000nm average transmittances are 0.044%.
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| CN111736253B (en) * | 2020-08-06 | 2020-11-20 | 上海翼捷工业安全设备股份有限公司 | CO2Infrared filter for gas detection and preparation method thereof |
| CN112162343B (en) * | 2020-11-02 | 2022-09-06 | 江西水晶光电有限公司 | Medium-far infrared filter for sensor and preparation method thereof |
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| CN113341491B (en) * | 2021-06-04 | 2022-05-17 | 微集电科技(苏州)有限公司 | Ultra-wide cut-off sulfur hexafluoride infrared filter and preparation method thereof |
| CN113608289B (en) * | 2021-08-05 | 2023-06-02 | 上海翼捷工业安全设备股份有限公司 | Infrared filter for nitrogen trifluoride gas detection and preparation method thereof |
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|---|---|---|---|---|
| DE3302565A1 (en) * | 1982-01-27 | 1983-08-11 | Kievskoe nauČno-proizvodstvennoe ob"edinenie "Analitpribor", Kiev | Frequency-limiting interference filter |
| CN202275177U (en) * | 2012-03-12 | 2012-06-13 | 杭州麦乐克电子科技有限公司 | 4260-nanometer band-pass infrared optical filter |
| CN104597549A (en) * | 2014-12-07 | 2015-05-06 | 杭州麦乐克电子科技有限公司 | 4600 nm band-pass infrared filtering sensitive element |
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- 2016-05-17 CN CN201610325524.7A patent/CN105842770B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3302565A1 (en) * | 1982-01-27 | 1983-08-11 | Kievskoe nauČno-proizvodstvennoe ob"edinenie "Analitpribor", Kiev | Frequency-limiting interference filter |
| CN202275177U (en) * | 2012-03-12 | 2012-06-13 | 杭州麦乐克电子科技有限公司 | 4260-nanometer band-pass infrared optical filter |
| CN104597549A (en) * | 2014-12-07 | 2015-05-06 | 杭州麦乐克电子科技有限公司 | 4600 nm band-pass infrared filtering sensitive element |
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