CN106125184A - A kind of formaldehyde gas detection infrared fileter and preparation method thereof - Google Patents
A kind of formaldehyde gas detection infrared fileter and preparation method thereof Download PDFInfo
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- CN106125184A CN106125184A CN201610778570.2A CN201610778570A CN106125184A CN 106125184 A CN106125184 A CN 106125184A CN 201610778570 A CN201610778570 A CN 201610778570A CN 106125184 A CN106125184 A CN 106125184A
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- film
- infrared fileter
- film system
- gas detection
- formaldehyde gas
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000001514 detection method Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000010408 film Substances 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 238000004062 sedimentation Methods 0.000 claims abstract description 11
- 239000010409 thin film Substances 0.000 claims abstract description 10
- 238000007747 plating Methods 0.000 claims abstract description 8
- 238000002834 transmittance Methods 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 230000008020 evaporation Effects 0.000 claims abstract description 6
- 229910021419 crystalline silicon Inorganic materials 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims abstract description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 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
- 238000000034 method Methods 0.000 claims description 28
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 16
- 230000003287 optical effect Effects 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 6
- 229910052732 germanium Inorganic materials 0.000 claims description 6
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 239000005083 Zinc sulfide Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- 238000000427 thin-film deposition Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 30
- 238000005485 electric heating Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000003969 polarography Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 229910052950 sphalerite Inorganic materials 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- QSLVNXFQCCTGET-UHFFFAOYSA-N benzene;hydrazine;hydrochloride Chemical compound Cl.NN.C1=CC=CC=C1 QSLVNXFQCCTGET-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
- 229960001553 phloroglucinol Drugs 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000004313 potentiometry Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating 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
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/28—Interference filters
- G02B5/285—Interference filters comprising deposited thin solid films
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a kind of formaldehyde gas detection infrared fileter and preparation method thereof, single crystalline Si selected by infrared fileter base material, and high-index material selects Ge, and ZnS selected by low-index material.Depositing main film system face thin film on two surfaces of substrate respectively and interfere cut film system face thin film, its coating process condition is that Ge selects electron beam evaporation plating, and sedimentation rate isZnS selects porous molybdenum boat electric heating evaporation, and sedimentation rate isStarting to be deposited with vacuum is 1.0 × 10‑3Pa, depositing temperature is 130 DEG C.The logical infrared fileter of 5768nm band that the present invention obtains, peak transmittance, up to more than 90%, improves signal to noise ratio greatly, well suppresses the interference of other gases, improves instrument detection accuracy and usefulness.
Description
Technical field
The present invention relates to a kind of infrared fileter production technology, be specifically related to a kind of formaldehyde gas detection infrared fileter
And preparation method thereof.
Background technology
Infrared-gas concentration detection principle is to measure gas concentration according to gas infrared signature absworption peak, therefore selects specific
The infrared gas analysis optical filter of wavelength is the critical component of infrared gas analyser.The light that light source sends after optical filter,
Obtain the quasi-monochromatic light (the narrowest degree of monochromaticity of bandwidth is the best) of certain bandwidth, after this light is actually taken up by gas by gas sample cell, by
Detector detection output intensity, thus extrapolate the concentration of gas.
In room air, textile, decorative materials, food, waste water, cosmetics and furniture etc., there is a large amount of formaldehyde gas
Body, but human body health and environmental pollution are caused the biggest impact as a kind of poisonous gas by formaldehyde gas.Therefore, I
National standard as an enforceable index and is implemented formaldehyde determination.
PARA FORMALDEHYDE PRILLS(91,95) detection method is broadly divided into chemical method and instrumental method two kinds the most both at home and abroad.Chemical method is broadly divided into: point
Light photometry (acetylacetone method, phenol reagent process, AHM T method, magenta-sulfurous method, off-color acid method, phloroglucinol method, hydrochloric acid benzene
Hydrazine method, enzyme process), Catalytic-Kinetic Spectrophotometric, fluorimetry.Instrumental method is broadly divided into: electrochemical process (differential (hydrargyrum is poor) pulse
Polarography, oscilloscopic polarography, potentiometry), chromatography (HPLC method, GC method, column chromatography) combination method (gas phase-mass spectrum (GC-MS)
Method, High Performance Liquid Chromatography/Mass Spectrometry (H PLC-MS) method, gas chromatogram-flame ionization detector (GC-FD) method, gas chromatogram-
Nitrogen phosphorous detector (GC-NPD) method, gas chromatography-electron capture detector (GC-ECD) method), sensor method.Chemical method has valency
Lattice are cheap, operate the advantages such as classical, easy to spread, but due to the principle of chemically based reaction, specificity is inadequate, is easily subject to phase
Interference like material;Though instrumental method has higher selectivity and higher sensitivity, but because it is expensive, cost is high, right
Operator's technology requires height, it is difficult to universal.
At present room, textile, food, the Formaldehyde In Cosmetics security incidents such as phenomenon that exceed standard occur again and again, not only affect
The quality of life of people, and Chinese commodity foreign trade added many obstacles.Therefore exploitation a kind of highly sensitive,
Selectivity is good, the logical infrared fileter of the band of good stability, accurate, economic formaldehyde gas is in good time and necessity, has certain
Realistic meaning and practical value widely.
Summary of the invention
The invention aims to solve above-mentioned the deficiencies in the prior art and provide a kind of peak transmittance high, can be greatly
Raising signal to noise ratio, effectively logical infrared fileter of 5768nm band of detection formaldehyde gas and preparation method thereof.
To achieve these goals, a kind of formaldehyde gas detection infrared fileter designed by the present invention, it is characterized in that:
(1) single crystalline Si is used to make substrate;Silicon twin polishing, thickness 300 ± 10 μm, crystal orientation<100>.
(2) Coating Materials selects zinc sulfide ZnS and monocrystalline germanium Ge, deposits main film system face respectively thin on two surfaces of substrate
Film and interference cut film system face thin film.
(3) main film system face membrane structure uses Sub/ (HL) 6H (LH) L (HL) 4H (LH) L (HL) 6H (LH) L/Air.
(4) cut film system face thin film is interfered to use: Sub/0.485 (HL)7 0.71(HL)7 1.4(HL)7/Air。
In film system, symbol implication is respectively as follows: Sub is substrate, and Air is air, H and L is respectively for surface film layer Ge (high index of refraction
Material layer) and 1/4 wave optical thickness of film layer ZnS (low refractive index material layer), central wavelength lambda=5768nm, 1H=
(4nHd)/λ;1L=(4nLD)/λ, the index during numeral is the thickness coefficient of film layer, structural formula in structural formula is membrane stack plated film
Periodicity.
The preparation method of above-mentioned a kind of formaldehyde gas detection infrared fileter, with monocrystal silicon Si as substrate, zinc sulfide
ZnS and germanium Ge is Coating Materials, uses the method for vacuum thermal evaporation thin film deposition to prepare film plating layer, and Ge selects electron beam evaporation plating,
Sedimentation rate is/sec;ZnS selects porous molybdenum boat electric heating evaporation, and sedimentation rate is/ sec, starts to be deposited with vacuum
It is 1.0 × 10-3Pa, depositing temperature is 130 DEG C.
The preparation method of above-mentioned a kind of formaldehyde gas detection infrared fileter, uses optical monitor to control film thickness
Degree, and it is aided with quartz-crystal control control sedimentation rate.
The above-mentioned logical infrared fileter of the 5768nm prepared band, main film system uses multi-cavity arrowband film structure, coordinates
The interference cut film system of the high cut-off degree of depth, centre wavelength is that 5768nm, 5700nm~5840nm wave band mean transmissivity is
91.87%, halfwidth is 190nm;In addition to the passband of centre wavelength 5768nm bandwidth 190nm, in the range of 2500~10000nm
Remaining spectrum all end, 2500~5600 average transmittance be 0.16%, 5940~10000 average transmittance be 0.3%,
Signal to noise ratio can be improved greatly, the interference of other gases, product optical property and physical strength energy can well be suppressed very well
Meet actual operation requirements, be widely used in formaldehyde gas infrared acquisition instrument, improve instrument detection accuracy and usefulness, permissible
Accomplish more rapid, confirm leakage point more accurately.
The present invention compared with prior art has the advantage that
1, optical filter is compared with traditional technology method, has the arrowband that centre wavelength is 5768nm and passes through spectrum, transmission bands
Rising edge and trailing edge precipitous, waveform rectangular degree is good, peak transmittance>90%, the cut-off degree of depth in cut-off region<0.3%, because of
Effective service band of this 5768nm can be the biggest pass through, the background noise of remaining invalid wave band is the most great
Reduce, thus the signal to noise ratio of excellence can be obtained, improve measurement sensitivity and the precision of instrument.
2, filter technology prepared by the present invention is simple, can form batch production, stable performance, meets high accuracy formaldehyde
The performance requirement of gas infrared acquisition instrument.
Accompanying drawing explanation
Fig. 1 is the structural representation of formaldehyde gas detection infrared fileter of the present invention.
Wherein: substrate 1 is single crystalline Si, film material 2 is Ge, and film material 3 is ZnS.
Fig. 2 is optical filter final performance measured curve figure.
Detailed description of the invention
The present invention is further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
As it is shown in figure 1, a kind of formaldehyde gas detection infrared fileter that the present embodiment provides is:
(1) single crystalline Si using a size of Φ 50.8 × 0.3mm makees substrate;Silicon twin polishing, thickness 300 ± 10 μm, brilliant
To<100>.
(2) Coating Materials selects zinc sulfide ZnS and monocrystalline germanium Ge, deposits main film system face respectively thin on two surfaces of substrate
Film A and interference cut film system face thin film B.
(3) main film system face thin film A uses: Sub/ (HL) 6H (LH) L (HL) 4H (LH) L (HL) 6H (LH) L/Air.
(4) cut film system face thin film B is interfered to use: Sub/0.485 (HL)7 0.71(HL)7 1.4(HL)7/Air。
In film system, symbol implication is respectively as follows: Sub is substrate, and Air is air, H and L is respectively for surface film layer 2 (Ge) (high refraction
Rate material layer) and 1/4 wave optical thickness of film layer 3 (ZnS) (low refractive index material layer), central wavelength lambda=5768nm,
1H=(4nHd)/λ;1L=(4nLD)/λ, the index during numeral is the thickness coefficient of film layer, structural formula in structural formula is membrane stack
The periodicity of plated film.
The preparation method of a kind of formaldehyde gas detection infrared fileter that the present embodiment provides, with germanium Ge as substrate, sulfur
Changing zinc ZnS and germanium Ge is Coating Materials, uses the method for vacuum thermal evaporation thin film deposition to prepare film plating layer, and Ge selects electron beam to steam
Plating, sedimentation rate is/sec;ZnS selects porous molybdenum boat electric heating evaporation, and sedimentation rate is / sec, starts to be deposited with vacuum
Degree is 1.0 × 10-3Pa, depositing temperature is 130 DEG C.
It is those skilled in the art institutes owing to specifically how to evaporate employing electron gun evaporation and employing resistance steaming evaporation coating
The routine techniques grasped, no further details to be given herein.
A kind of this patent optical filter that the present embodiment provides uses one side to plate multi-cavity arrowband film system, improves effective service band
Transmitance and waveform rectangular degree, once improve valid signal strengths;The interference cut film system of the another side plating height cut-off degree of depth, arrives
Reach all invalid secondary peak in addition to passband in the range of 2500~10000nm.
The present embodiment provide formaldehyde gas detection infrared fileter, its centre wavelength positioning precision within 0.7%,
Film system uses optical monitor control thicknesses of layers, and is aided with quartz-crystal control control sedimentation rate.
Use Bruker company of Germany VERTEX 70 type Fourier infrared spectrograph that prepared optical filter is surveyed
Examination.The optical filter final performance measured curve figure of this optical filter final performance structure such as Fig. 2:
1. central wavelength lambda=5768nm;
2. bandwidth Delta lambda=190nm;
3. form factor Δ λ 10%/Δ λ 50%=1.42;
4. peak transmittance Tp=91.87%
1500-10000nm T in addition to passbandavg≤ 0.3%.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention, every according to the present invention
Any simple modification, change and the equivalent structure transformation that above example is made by technical spirit, all still falls within skill of the present invention
In the protection domain of art scheme.
Claims (4)
1. a formaldehyde gas detection infrared fileter, it is characterised in that:
(1) single crystalline Si is used to make substrate;Silicon twin polishing, thickness 300 ± 10 μm, crystal orientation<100>;
(2) Coating Materials select zinc sulfide ZnS and monocrystalline germanium Ge, two surfaces of substrate deposit respectively main film system face thin film and
Interfere cut film system face thin film;
(3) main film system face membrane structure uses Sub/ (HL) 6H (LH) L (HL) 4H (LH) L (HL) 6H (LH) L/Air;
(4) cut film system face thin film is interfered to use: Sub/0.485 (HL)70.71(HL)71.4(HL)7/Air;
In film system, symbol implication is respectively as follows: Sub is substrate, and Air is air, H and L is respectively for surface film layer Ge (high-index material
Layer) and 1/4 wave optical thickness of film layer ZnS (low refractive index material layer), central wavelength lambda=5768nm, 1H=
(4nHd)/λ;1L=(4nLD)/λ, the index during numeral is the thickness coefficient of film layer, structural formula in structural formula is membrane stack plated film
Periodicity.
2. a kind of formaldehyde gas detection infrared fileter as claimed in claim 1, it is characterised in that: use vacuum thermal evaporation
The method of thin film deposition prepares film plating layer, and Ge selects electron beam evaporation plating, and sedimentation rate isZnS selects porous molybdenum boat electricity
Heat evaporation, sedimentation rate isStarting to be deposited with vacuum is 1.0 × 10-3Pa, depositing temperature is 130 DEG C.
3. a kind of formaldehyde gas detection infrared fileter as claimed in claim 2, it is characterised in that: use optical monitor
Control thicknesses of layers, and be aided with quartz-crystal control control sedimentation rate.
4. a kind of formaldehyde gas detection infrared fileter as claimed in claim 1, it is characterised in that: described infrared filtering
Sheet, main film system uses multi-cavity arrowband film structure, coordinates the interference cut film system of the height cut-off degree of depth, and centre wavelength is 5768nm,
5700nm~5840nm wave band mean transmissivity is 91.87%, and halfwidth is 190nm;Except centre wavelength 5768nm bandwidth 190nm
Passband outside, remaining spectrum in the range of 2500~10000nm all ends, and 2500~5600 average transmittance are
0.16%, 5940~10000 average transmittance is 0.3%.
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Cited By (2)
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CN111323861A (en) * | 2020-05-13 | 2020-06-23 | 翼捷安全设备(昆山)有限公司 | Infrared filter for acetylene gas detection, preparation method and application thereof |
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CN110261949A (en) * | 2019-06-25 | 2019-09-20 | 镇江爱豪科思电子科技有限公司 | A kind of sulfur dioxide gas detection infrared fileter and preparation method thereof |
CN110261949B (en) * | 2019-06-25 | 2021-10-15 | 镇江爱豪科思电子科技有限公司 | Infrared filter for detecting sulfur dioxide gas and preparation method thereof |
CN111323861A (en) * | 2020-05-13 | 2020-06-23 | 翼捷安全设备(昆山)有限公司 | Infrared filter for acetylene gas detection, preparation method and application thereof |
CN111323861B (en) * | 2020-05-13 | 2021-12-03 | 翼捷安全设备(昆山)有限公司 | Infrared filter for acetylene gas detection, preparation method and application thereof |
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