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 PDF

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Publication number
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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CN106125184B (en
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刘桂武
张旭
邵海成
侯海港
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Zhenjiang Aihaokesi Electronic Technology Co Ltd
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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

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  • 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

A kind of formaldehyde gas detection infrared fileter and preparation method thereof
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%.
CN201610778570.2A 2016-08-30 2016-08-30 A kind of formaldehyde gas detection infrared fileter and preparation method thereof Active CN106125184B (en)

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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
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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Publication number Priority date Publication date Assignee Title
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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