CN106596451A - Method for producing light source of non dispersive infrared spectrum gas analyzer - Google Patents

Method for producing light source of non dispersive infrared spectrum gas analyzer Download PDF

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Publication number
CN106596451A
CN106596451A CN201611217635.2A CN201611217635A CN106596451A CN 106596451 A CN106596451 A CN 106596451A CN 201611217635 A CN201611217635 A CN 201611217635A CN 106596451 A CN106596451 A CN 106596451A
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light source
thin film
chip
platinum
preparation
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Inventor
任兴平
刘宇翔
张建红
杨红飞
崔茂荣
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KUNMING SIPAITE SPECTRUM TECHNOLOGY CO LTD
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KUNMING SIPAITE SPECTRUM TECHNOLOGY CO LTD
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    • 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
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00Features of devices classified in G01N21/00
    • G01N2201/06Illumination; Optics
    • G01N2201/061Sources
    • G01N2201/06186Resistance heated; wire sources; lamelle sources

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  • Physics & Mathematics (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)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention discloses a method for producing a light source of a non dispersive infrared spectrum gas analyzer, and the method comprises preparation of a thermal insulating film, preparation of an electrode pad film, preparation of a thermal resistance film, preparation of a light source chip, integration of the light source chip and a light source signal processing circuit and preparation of the light source. The method aims at the technical problems of poor system signal noise ratio and low detection sensitivity for the reason that a spectrum gas analyzer in the prior art can only work in a low frequency, the light source prepared by the method can work in the condition of a high frequency, can be used in design and production of anon dispersive gas analyzer based on the principle of spectrum absorption, and further can be used in field of online monitoring of toxic and harmful gases.

Description

A kind of light source preparation method of on-dispersive type infrared spectrum gas analyser
Technical field
The present invention relates to a kind of light source preparation method of on-dispersive type infrared spectrum gas analyser, belongs to light source and makes neck Domain.
Background technology
Toxic and harmful analyser based on spectrographic method is mainly used at present industry, agricultural, medical treatment, intelligence The industries such as energy building, analytical tool are used for the high accuracy of gas concentration and survey, and are such as used in pollutant monitoring, tailstock edema caused by disorder of QI Analysis, gas and combustible gas detection, gas composition analysis, medical monitoring device, air quality analysis, elementary analysiss instrument etc. are led Domain.Spectroscopy gas analyser is a kind of instrument of measure spectra Absorption spectra, and the instrument of this type is required for launch continuous The light source of spectral radiance and sensitive spectroscopic detector.
One of core devices of spectroscopy gas analyser are spectroscopic detectors.In general, pyroelectric detector is red The preferable selection of spectroscopic detector in the development of external spectrum method gas analyser.The sensitivity of pyroelectric detector and response frequency it Between relation it is very complicated, it is not a simple linear relationship or can be described with a simple equation.Typically Ground says that to improve sensitivity will sacrifice response frequency, and improving response frequency, then to reduce the time of integration sensitive so as to lose Degree.However, being not that relation on all of frequency band between device sensitivity and response frequency all follows such rule. Complex physical problem is forgiven in the middle of this.Pyroelectric detector has two types, and a kind of is film type, with thin film material Expect for light-sensitive material, frequency band when its device voltage responsiveness reaches maximum is typically in 10Hz-100Hz;Another kind is pottery Porcelain type, with ceramic material as light-sensitive material, frequency band when its device voltage responsiveness reaches maximum is typically in 0.1Hz- 1Hz.But either which kind of type, its noise and frequency are all related, and in low frequency, noise is very big, and the noise in high frequency Very big, it is very big that this is primarily due to white noise during low frequency.It is to pursue larger voltage in the design of spectroscopy gas analyser Signal, when answering selector voltage responsibility to reach maximum or its adnexa frequency as pyroelectric detector work frequency Rate, this frequency is actually the modulating frequency that electric ac modulation is carried out to light source.It is obvious that the modulating frequency of light source is set Meter selects film type pyroelectric detector to be that spectroscopic detector will make system obtain maximum signal to noise ratio, while also in high band Optimal detection sensitivity will be obtained.The precondition for realizing this design is exactly that light source will have response frequency faster.
The two of the core devices of spectroscopy gas analyser are the light sources that can launch continuous radiation.Light source is by adding A kind of inert solid of heat produces radiation.The temperature of hot solid is generally 1500~2200K, maximum radiant intensity 5000~ Between 5900cm-1.Mainly there are siliconits and Nernst glower in the more practical infrared light supply of middle infrared at present.Siliconits are by carbon SiClx sintering is formed.Its radiation intensity distribution deflection long wave, operating temperature is generally 1300~1500K.Because carborundum has liter Magnificent phenomenon, using temperature is too high the life-span of carborundum will be shortened, and can pollute neighbouring dyeing mirror.Siliconits light-emitting area is big, Low price, it is easy to operate, using wave-length coverage compared with Nernst glower width.Nernst glower mainly by mix rare earth metal (zirconium, Thorium, cerium) oxide makes.It has negative temperature-coefficient of electrical resistance, is at room temperature non-conductor, when temperature is increased to about 500 DEG C During the above, it is changed into quasiconductor, when more than 700 DEG C, just becomes conductor.Therefore Nernst glower is lighted, is needed in advance its is pre- Heat is to 700 DEG C.Its operating temperature is typically at 1750 DEG C.Nernst glower service life is longer, and good stability is used in short wave ranges It is more favourable than siliconits.But its is expensive, operate be not as convenient as siliconits.In 50 μm of far red light areas of λ >, need using high Pressure mercury lamp.Tengsten lamp is generally adopted in the near-infrared region of 20000~8000cm-1.In the concentration for monitoring some atmosphere pollutions With the absorbing material determined in aqueous solution (such as:Ammonia, butadiene, benzene, ethanol, nitrogen dioxide and trichloro ethylene etc.) when, can adopt With adjustable carbon dioxide laser light source.Its radiant intensity several orders of magnitude bigger than blackbody source.Above light source is due to volume It is larger and price is higher, in can be only applied to the spectrum analyses of laboratory.
At present the spectroscopy gas analyser of on-line monitoring is typically with the common microminiature bulb with tungsten filament as heater As light source.The advantage of this light source is low cost, but technically has the too long of shortcoming of response time, and it is in higher modulation The spectral energy exported under frequency is too low, can only work under low frequency modulations, it is impossible to the spectrum inspection that can be worked in high frequency Survey device such as film type pyroelectric detector to use cooperatively to reach optimal signal to noise ratio, so that the inspection of spectroscopy gas analyser Survey sensitivity to be difficult to get a promotion.
The content of the invention
In order to solve spectroscopy gas analyser present in prior art can only work at low frequency institute caused by a system The technical problem that noise is poor and detection sensitivity is relatively low, the present invention proposes a kind of on-dispersive type infrared spectrum gas analyses The light source preparation method of instrument can be worked using the light source that the method makes under high frequency condition, can be based on Spectrum Absorption Principle On-dispersive type gas analyser design and used in making, and then answered in the on-line monitoring field of toxic and harmful With.
A kind of light source preparation method of on-dispersive type infrared spectrum gas analyser proposed by the present invention, the method is as follows What step was realized:
Step one:Heat insulation thin film is prepared on the single crystal silicon substrate for crossing silicon dioxide insulator thin film;
The porous that prepare one layer inorganic-organic hybridization has been coated with the single crystal silicon substrate of silicon dioxide insulator thin film on surface SiO2Thin film, the area of described single crystal silicon substrate can be Φ 10mm- Φ 100mm, the porous of the inorganic-organic hybridization of preparation SiO2Film thickness is 2 μm -6 μm.
Step 2:Electrode pressure welding block is prepared on heat insulation thin film;
Using many target direct current magnetron sputtering process inorganic-organic hybridization porous SiO2Platinum/titanium is prepared on thin film thin Film simultaneously adopts positive glue stripping method according to the patent of Application No. 200510010975.3:A kind of Pt/Ti metal membrane patterning technique Described method is completed graphically;Wherein, the size dimension of each light source chip determines according to actual needs,
The thickness of the platinum/platinum/titanium metal thin film is 100nm-1000nm, and size dimension is in the range of Φ 0.5mm- Φ 2mm.
Step 3:On heat insulation thin film between two electrode pressure welding blocks, amorphous carbon or carborundum films conduct are prepared Heat resistive film, and completed graphically using dry and wet etch;
Carborundum films are prepared as heat on platinum/platinum/titanium metal thin film using plasma-reinforced chemical sedimentation (PECVD) Resistance thin film is simultaneously completed graphically using dry and wet etch, and the thickness of described heat resistive film is 300nm-1000nm;Carbon SiClx heat resistive film thickness is 800nm, this thin film two ends connection electrode, meanwhile, the thin film it is graphical after in continuous bow word Shape, the line thickness for bending font is 100-200 μm, and the gap between adjacent parallel wales is 10-50 μm.
Step 4:Scribing is carried out to light source chip, the light source chip after scribing is connected with process circuit and is packaged;
Using scribing machine, knife completes scribing under the intersection of each light source chip, from the silicon chip of full wafer 20mm × 20mm 16 same sheet laser chips are obtained, and completes the welding between one end of chip link and chip pressure welding block.
Chip is bonded together with signal processing circuit board, and completes the other end and and letter benefit reason of chip link The welding of circuit board leads, obtains light source chip component.
The shell encapsulation of light source chip component, band spectrum window and base is completed into the making of light source.
The invention has the beneficial effects as follows:
1st, the present invention is generated heat using amorphous carbon or carborundum films as heat resistive film material after electric current, generation Spectral radiance.There is its thermal resistance material characteristic high emissivity to work under continuous operation mode and pulse mode, can meet Spectrum sends out performance requirement of the gas analyser to light source.
2nd, the present invention prepares heat resistive film using amorphous carbon or carborundum films as heat resistive film using silicon planner technology Chip, with very low hot residence characteristics, makes it when high-frequency impulse works, and quick can must heat and cool down, quick response, light Source can be performed for more than the modulation (30Hz modulating frequencies are in 50% dutycycle) of 100Hz, be conducive to sending out gas analyser in spectrum The characteristics of low noise under senior engineer's working frequency being played in development.
Description of the drawings
Fig. 1 is for the light source preparation flow figure of on-dispersive type spectroscopic gas analyser;
Fig. 2 is that heat insulation thin film prepares schematic diagram in embodiment;
Fig. 3 is that light source cell electrode pressure welding block thin film prepares schematic diagram in embodiment;
Fig. 4 is that heat resistive film prepares schematic diagram in embodiment.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention will be described in detail.
A kind of light source preparation method of on-dispersive type infrared spectrum gas analyser, as described in Figure 1, the concrete party of realization The step of method is realized is as follows:
Step one:Heat insulation thin film is prepared on the single crystal silicon substrate for crossing silicon dioxide insulator thin film;
The porous that prepare one layer inorganic-organic hybridization has been coated with the single crystal silicon substrate of silicon dioxide insulator thin film on surface SiO2Thin film, the area of described single crystal silicon substrate can be Φ 10mm- Φ 100mm, the porous of the inorganic-organic hybridization of preparation SiO2 film thicknesses are 2 μm -6 μm.
In the present embodiment, it is 20mm × 20mm to take one piece of area, and surface is coated with 1 μ m thick silicon dioxide insulator thin film, Crystal orientation is《100》The thickness in direction is 300 μm of silicon single crystal matrix.1 μ m thick SiO is coated with it2Insulation film that Porous SiO of the inorganic-organic hybridization that a layer thickness is 3 μm is prepared in layer surface2Thin film, as shown in Figure 2.
Step 2:Electrode pressure welding block is prepared on heat insulation thin film;
Using many target direct current magnetron sputtering process inorganic-organic hybridization porous SiO2Platinum/titanium is prepared on thin film thin Film simultaneously adopts positive glue stripping method according to the patent of Application No. 200510010975.3:A kind of Pt/Ti metal membrane patterning technique Described method is completed graphically;Wherein, the size dimension of each light source chip determines according to actual needs,
The thickness of the platinum/platinum/titanium metal thin film is 100nm-1000nm, and size dimension is in the range of Φ 0.5mm- Φ 2mm;
In the present embodiment, using many target direct current magnetron sputtering process, in the porous sio2 for preparing inorganic-organic hybridization It is a unit by area 5mm × 5mm on the silicon single crystal flake of thin film, in its upper left corner and the lower right corner 1 electrode pressure welding is respectively prepared Block (i.e. platinum/titanium) thin film, thickness is 800nm, and size is 1mm × 1mm.
Platinum/platinum/titanium metal thin film graphically using positive glue stripping method according to patent:A kind of Pt/Ti metal membrane patterning skill Art (the patent No.:ZL 200510010975.3) described in method complete graphically.Electrode pressure welding block thin film is that platinum/titanium is thin The thickness of film is 800nm, and its size dimension is 1mm × 1mm.The size dimension of each light source chip is 5mm × 5mm, each The figure of the electrode pressure welding block thin film of the light source chip of individual unit is as shown in Figure 3.
Wherein many target direct current magnetron sputtering process grow the process conditions such as table 1 of platinum/platinum/titanium metal thin film:
Table 1:Many target direct current magnetron sputtering process grow platinum/platinum/titanium metal thin film process conditions
Power Target size Carrier gas Target-substrate distance The pre-sputtering time Growth time
Titanium target 80W Φ60mm Argon 70mm 60s 30s
Platinum target 80W Φ60mm Argon 70mm 60s 120s
The slice, thin piece after platinum/platinum/titanium metal thin film prepares and be graphical will be completed to be put in quick anneal oven, and by such as table 2 below Described process conditions carry out heat treatment:
Table 2:Platinum:/ platinum/titanium metal thin film heat treatment condition
Heating rate Annealing temperature Temperature retention time
50℃/s 550℃ 300s
Step 3:On heat insulation thin film between two electrode pressure welding blocks, amorphous carbon or carborundum films conduct are prepared Heat resistive film, and completed graphically using dry and wet etch;
Carborundum films are prepared as heat on platinum/platinum/titanium metal thin film using plasma-reinforced chemical sedimentation (PECVD) Resistance thin film is simultaneously completed graphically using dry and wet etch, and the thickness of described heat resistive film is 300nm-1000nm;Carbon SiClx heat resistive film thickness is 800nm, this thin film two ends connection electrode, meanwhile, the thin film it is graphical after in continuous bow word Shape, the line thickness for bending font is 100-200 μm, and the gap between adjacent parallel wales is 10-50 μm.
The wherein process conditions of plasma-reinforced chemical sedimentation (PECVD) growing silicon carbide film such as table 3:
Table 3:Plasma-reinforced chemical sedimentation (PECVD) growing silicon carbide film process conditions
Carrier gas Power Working gas 1 Working gas 2 Growth time
Argon 300W Silane SiH4 Methane CH4 2 hours
The removal technique of the carborundum films in the patterning process of carborundum films sends out etching method (reactive ion using dry Etching method):Its process conditions such as table 4:
Table 4:Reactive ion etching method removes carborundum films process conditions
Carrier gas Power Reacting gas Etch period
Argon 200W Sulfur hexafluoride SF6 1 hour
Step 4:Scribing is carried out to light source chip, the light source chip after scribing is connected with process circuit and is packaged;
Using scribing machine, knife completes scribing under the intersection of each light source chip, from the silicon chip of full wafer 20mm × 20mm 16 same sheet laser chips are obtained, and complete the welding between one end of chip link and chip pressure welding block,
Chip is bonded together with signal processing circuit board, and completes the other end and and letter benefit reason of chip link The welding of circuit board leads, obtains light source chip component, is by the shell encapsulation of light source chip component, band spectrum window and base Complete the making of light source.
The ultimate principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry Personnel it should be appreciated that the present invention is not restricted to the described embodiments, the simply explanation described in above-described embodiment and description this The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes Change and improvement is both fallen within scope of the claimed invention.The claimed scope of the invention by appending claims and its Equivalent thereof.

Claims (1)

1. a kind of light source preparation method of on-dispersive type infrared spectrum gas analyser, the method is the steps of what is realized:
Step one:Heat insulation thin film is prepared on the single crystal silicon substrate for crossing silicon dioxide insulator thin film;
The porous sio2 that prepare one layer inorganic-organic hybridization has been coated with the single crystal silicon substrate of silicon dioxide insulator thin film on surface Thin film, the area of described single crystal silicon substrate can be Φ 10mm- Φ 100mm, and the porous sio2 of the inorganic-organic hybridization of preparation is thin Film thickness is 2 μm -6 μm.
Step 2:Electrode pressure welding block is prepared on heat insulation thin film;
Platinum/platinum/titanium metal thin film is prepared using many target direct current magnetron sputtering process simultaneously on the porous sio2 thin film of inorganic-organic hybridization Using positive glue stripping method according to Application No. 200510010975.3 patent:Described in a kind of Pt/Ti metal membrane patterning technique Method complete graphically;Wherein, the size dimension of each light source chip determines according to actual needs,
The thickness of the platinum/platinum/titanium metal thin film is 100nm-1000nm, and size dimension is in the range of Φ 0.5mm- Φ 2mm;
Step 3:On heat insulation thin film between two electrode pressure welding blocks, amorphous carbon or carborundum films are prepared as thermal resistance Thin film, and completed graphically using dry and wet etch;
Carborundum films are prepared on platinum/platinum/titanium metal thin film using plasma-reinforced chemical sedimentation (PECVD) thin as thermal resistance Film is simultaneously completed graphically using dry and wet etch, and the thickness of described heat resistive film is 300nm-1000nm;Carborundum Heat resistive film thickness is 800nm, this thin film two ends connection electrode, meanwhile, the thin film it is graphical after in continuous bow font, bow The line thickness of font is 100-200 μm, and the gap between adjacent parallel wales is 10-50 μm;
Step 4:Scribing is carried out to light source chip, the light source chip after scribing is connected with process circuit and is packaged;
Using scribing machine, knife completes scribing under the intersection of each light source chip, obtains from the silicon chip of full wafer 20mm × 20mm 16 same sheet laser chips, and complete the welding between one end of chip link and chip pressure welding block;
Chip is bonded together with signal processing circuit board, and complete the other end of chip link with and believed process circuit The welding of plate lead, obtains light source chip component, and the shell encapsulation of light source chip component, band spectrum window and base is completed The making of light source.
CN201611217635.2A 2016-12-26 2016-12-26 Method for producing light source of non dispersive infrared spectrum gas analyzer Pending CN106596451A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109799206A (en) * 2019-03-08 2019-05-24 上海大学 A kind of overstepping one's bounds light type infrared gas sensor and its method of operation

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202165999U (en) * 2011-03-09 2012-03-14 李小玲 LED (Light-emitting Diode) light source with beautifying and lighting functions
CN102621109A (en) * 2012-03-06 2012-08-01 昆明斯派特光谱科技有限责任公司 Light source preparation method for nondispersive spectrum gas analysis instrument
CN103700654A (en) * 2013-12-20 2014-04-02 纳晶科技股份有限公司 LED (Light-Emitting Diode) based on COB (Chip On Board) package and manufacturing method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202165999U (en) * 2011-03-09 2012-03-14 李小玲 LED (Light-emitting Diode) light source with beautifying and lighting functions
CN102621109A (en) * 2012-03-06 2012-08-01 昆明斯派特光谱科技有限责任公司 Light source preparation method for nondispersive spectrum gas analysis instrument
CN103700654A (en) * 2013-12-20 2014-04-02 纳晶科技股份有限公司 LED (Light-Emitting Diode) based on COB (Chip On Board) package and manufacturing method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109799206A (en) * 2019-03-08 2019-05-24 上海大学 A kind of overstepping one's bounds light type infrared gas sensor and its method of operation

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Application publication date: 20170426