CN112798536B - Integrated miniature gas absorption tank - Google Patents
Integrated miniature gas absorption tank Download PDFInfo
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- CN112798536B CN112798536B CN202011614221.XA CN202011614221A CN112798536B CN 112798536 B CN112798536 B CN 112798536B CN 202011614221 A CN202011614221 A CN 202011614221A CN 112798536 B CN112798536 B CN 112798536B
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
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- G—PHYSICS
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- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G01N2021/0339—Holders for solids, powders
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- G—PHYSICS
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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G01N2021/0346—Capillary cells; Microcells
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Abstract
The invention discloses an integrated micro gas absorption cell, which comprises a top plate, a bottom plate, two reflector-micro-nano lens integrated elements and two sealing plates, wherein the two reflector-micro-nano lens integrated elements and the two sealing plates are arranged between the top plate and the bottom plate; the top plate and the bottom plate are provided with vent holes; the two reflector-micro-nano lens integrated elements consist of a transparent substrate, a super-surface lens and a reflector which are arranged on the front surface of the transparent substrate, and an antireflection film arranged on the back surface of the transparent substrate, wherein the front surface of the transparent substrate faces the inside of the absorption cell; the two reflectors and the micro-nano lens integrated element are arranged oppositely, the two super-surface lenses are staggered with each other, and the outer sides of the super-surface lenses are respectively provided with an adjustable laser and a detector. The two super surface lenses can also be arranged on any one of the two reflector-micro nano lens integrated elements. The invention can effectively solve the problems that the existing gas absorption cell has larger volume and higher cost and is difficult to realize high-precision alignment packaging because each key optical element is separated.
Description
Technical Field
The invention belongs to the field of gas detection, relates to a gas detection and concentration analysis device, and particularly relates to an integrated miniature gas absorption cell.
Background
The analysis of the gas types and the gas concentrations is widely applied to the fields of home, security, quality inspection, scientific research and the like. Since each molecule has different characteristic absorption peaks for light, spectral analysis becomes a powerful means for qualitative and quantitative analysis of gases. Gas absorption cells are common tools for the detection of gas components using spectroscopic analysis. The gas to be detected is introduced into the gas absorption cell, a beam of laser is introduced into the gas absorption cell, the laser penetrates through the gas to be detected and interacts with the gas to be detected, then the laser is received by the detector or the spectrometer, and the type and the concentration of the gas in the cell can be determined by analyzing the spectrum and the intensity of the received light. To ensure the accuracy of the detection, the light needs to have a sufficiently long interaction distance with the gas to be detected. Therefore, a set of opposing mirrors is required to reflect light back and forth within the cell to increase the optical path length of the gas within the cell, and accordingly, optical components are required to shape and control the light beam in order to ensure that the light energy reflected multiple times is accurately coupled into the detection device. The current gas absorption cell technology is mainly based on the forms of a White White cell, a Herriott cell and the like, and various components such as a reflector, a lens and the like of the gas absorption cells are separated, so that the coupling alignment difficulty is high, the volume is large, and the gas inlet and outlet speed is limited; in addition, the problems of high cost, poor stability and the like are brought to the existing gas absorption cell, and the large-scale deployment of the gas detection technology is limited. Therefore, the biggest problem of the gas absorption cell technology is how to realize miniaturization and high-precision and low-cost packaging so as to produce a stable, reliable and low-cost gas absorption cell and break application bottlenecks.
Disclosure of Invention
The invention aims to provide an ultra-small optical gas absorption cell, which can effectively solve the problems that the conventional gas absorption cell has larger volume and higher cost and is difficult to realize high-precision alignment packaging because each key optical element is separated.
The technical scheme adopted by the invention is as follows:
an integrated micro gas absorption cell comprises a top plate, a bottom plate, two reflector-micro nano lens integrated elements and two sealing plates, wherein the two reflector-micro nano lens integrated elements and the two sealing plates are arranged between the top plate and the bottom plate;
the top plate and the bottom plate are provided with vent holes for the inlet and outlet of gas;
the two reflector-micro-nano lens integrated elements are composed of a transparent substrate, a micro-nano lens and a reflector which are arranged on the front surface of the transparent substrate and an antireflection film arranged on the back surface of the transparent substrate, wherein the front surface of the transparent substrate faces the inside of the absorption pool, and the back surface of the transparent substrate faces the outside of the absorption pool; the micro-nano lens is a super-surface lens realized by adopting a super-surface technology; the two reflector-micro nano lens integrated elements are oppositely arranged, and the two super surface lenses are staggered with each other; the outer sides of the super-surface lenses of the two reflector-micro-nano lens integrated elements are respectively provided with an adjustable laser and a detector;
and sealing joints of all the components after the gas absorption cell is assembled.
In the above technical solution, further, the reflector may be any one of a metal reflector, a multilayer dielectric thin film reflector, a diffraction structure reflector, or a super surface material reflector.
Furthermore, the super-surface lens is arranged at one end of the reflector-micro-nano lens integrated element.
Furthermore, the reflector-micro-nano lens integrated element integrally prepares the lens and the reflector through a semiconductor process, and realizes accurate alignment of the optical axis of the lens and the optical axis of the reflector.
Further, the transparent substrate is made of a hard material which is non-absorptive to the wavelength of the detection laser, and includes but is not limited to quartz, sapphire, calcium fluoride, silicon, germanium or chalcogenide glass, and the transparent substrate is integrated with an electrical interconnection line for providing electrical interconnection for power supply and control of the tunable laser and the detector.
Furthermore, the vent holes are filled with filter materials for suspending particulate matters and specific gas molecules.
Furthermore, a reflector limiting clamping groove and a sealing plate limiting clamping groove are formed in the top plate and the bottom plate and are respectively used for fixing the reflector-micro-nano lens integrated element and the sealing plate, and an adjustable laser clamping groove and a detector clamping groove are also formed in the top plate and are respectively used for fixing an adjustable laser and a detector.
Furthermore, the top plate and the bottom plate are processed from silicon wafers, and the reflector limiting clamping groove, the sealing plate limiting clamping groove and the vent hole are all prepared by utilizing photoetching and deep silicon etching processes.
The invention also provides an integrated micro gas absorption cell which is different from the structure, and the structure of the absorption cell is different from that of the absorption cell in claim 1 in that in the two reflector-micro nano lens integrated elements:
one reflector-micro-nano lens integrated element consists of a transparent substrate, a reflector arranged on the front surface of the transparent substrate and an antireflection film arranged on the back surface of the transparent substrate;
the other reflector-micro-nano lens integrated element consists of a transparent substrate, micro-nano lenses and reflectors which are arranged on the front surface of the transparent substrate, and an antireflection film arranged on the back surface of the transparent substrate, wherein the number of the micro-nano lenses arranged on the front surface of the transparent substrate is two, and the two micro-nano lenses are respectively arranged at two ends of the transparent substrate. The micro-nano lens is a super-surface lens realized by adopting a super-surface technology.
In the reflector-micro-nano lens integrated element, reflectors are arranged at other positions except the position of the super-surface lens on the front surface of the transparent substrate.
The invention principle of the invention is as follows:
the invention provides an integrated micro gas absorption cell based on micro-nano processing by utilizing a semiconductor process. The lens and the reflector are integrally prepared through a semiconductor process, so that the optical axis of the lens and the optical axis of the reflector are accurately aligned; the optical path folding is carried out through back-and-forth reflection by the aid of the two-sided reflector and the ultra-small incident angle, so that the interaction distance between meter-level light and gas molecules is obtained, and ultrahigh detection sensitivity is obtained; the light collection and alignment through the micro gas absorption cell are realized by using the integrated super-surface lens at the receiving end; meanwhile, the semiconductor technology is utilized to precisely process the packaging module clamp, so that precise clamping alignment is realized, and the packaging difficulty, time and cost are greatly reduced; the vent holes are reserved through the packaging clamp, particles and specific gas filtering or enriching materials are filled in the vent holes, and rapid real-time or trace gas concentration detection is achieved. The technical scheme can realize the ultra-small gas absorption cell, realize batch preparation by utilizing the semiconductor process, and completely fix the structural light path, meet the requirements of quick, low-cost and high-precision packaging, thereby greatly reducing the cost of the high-sensitivity gas sensor and being beneficial to large-scale batch deployment.
Compared with the prior art, the invention has the beneficial effects that:
1) all the lenses and the reflecting mirror are integrated by utilizing a semiconductor technology, so that the volume of the gas absorption cell is obviously reduced, high-sensitivity gas sensing can be realized, and the assembly cost is reduced.
2) The position of the reflector-micro nano lens integrated element can reach micron level by utilizing the limit groove manufactured by the semiconductor process, and the gas absorption cell can be fully integrated with components such as a laser, a detector and the like in an expanded manner, so that the mutual alignment difficulty of the packaging components is greatly reduced, and the packaging time and cost are greatly reduced.
3) The design of the gas absorption cell provided by the invention can be suitable for visible mid-infrared wave bands, thereby meeting the requirements of different gas component analysis.
Drawings
FIG. 1 is a schematic diagram of a reflector-micro-nano lens integrated element of a gas absorption cell;
FIG. 2 is a schematic view of the floor/ceiling structure of a gas absorption cell;
FIG. 3(A) is a schematic view of the overall structure of a gas absorption cell; FIG. 3(B) is a schematic diagram showing the transmission of light in the gas absorption cell shown in FIG. 3 (A);
FIG. 4(A) is a schematic view showing the entire structure of the integrated micro gas absorption cell, and FIG. 4(B) is a sectional view taken along the line B-B of the top plate in FIG. 4 (A);
FIG. 5(A) is a schematic view of the entire structure of embodiment 3; FIG. 5(B) is a schematic diagram showing the transmission of light in the gas absorption cell shown in FIG. 5 (A);
wherein 001 is a reflector-micro-nano lens integrated element, 002 is a top plate, 003 is a sealing plate, 004 is a bottom plate, 101 is a transparent substrate, 102 is a reflector, 103 is a super-surface lens, and 104 is an antireflection film; 202-1 is a reflector limiting clamping groove, 202-2 is a sealing plate limiting clamping groove, 203 is an air vent, 301 is a light source, 302 is a light detection device, 401 is a tunable laser, 401-1 is a laser clamping groove, 402 is a detector, and 402-1 is a detector clamping groove.
Detailed Description
The following further illustrates the invention by means of specific examples, which should not be construed as in any way limiting the scope of the invention.
An integrated micro gas absorption cell is schematically shown in fig. 4. In this embodiment, a tunable laser 401 and a detector 402 are co-integrated with a gas absorption cell (see fig. 4 (a)).
The substrate material of the reflector-micro-nano lens integrated element 001 is a quartz wafer, the super-surface lens 103 and the high-contrast grating reflector 102 are integrated on the upper front surface of the substrate material, the anti-reflection film 104 is plated on the back surface of the substrate material, the working wavelength range of the super-surface lens 103, the reflector 102 and the anti-reflection film 104 is 1700nm, wherein the NA of the silicon-based super-surface lens is 0.2 or 0.5, the reflectivity of the reflector is more than 99%, the overall length is 1-3cm, the width is 300-1000 microns, the size of the micro-lens is 100-500 microns, and the monolithic integration of the lens and the reflector is carried out by utilizing a semiconductor thin film deposition and etching process.
Fig. 4(B) is a B-B sectional view of the top plate 002. The top plate 002/bottom plate 004 is formed by processing a 800-micron thick silicon wafer, the reflector limiting clamping groove 202-1, the sealing plate limiting clamping groove 202-2 and the vent hole 203 are all prepared by utilizing photoetching and deep silicon etching processes, and the depth of the clamping groove is 100-300 microns. The reflector limiting clamping groove 202-1 is used for fixing the reflector-micro-nano lens integrated element 001, the laser clamping groove 401-1 is used for fixing the adjustable laser (VCSEL vertical cavity surface emitting adjustable laser) 401, the detector clamping groove 402-1 is used for fixing the InGaAs detector 402, and the sealing plate limiting clamping groove 202-2 is used for fixing the sealing plate 003 and sealing the joint of each element after assembly. The clamping grooves can realize micron-scale accurate alignment from a light source to a detector and a folding optical path device, emergent light of a laser can be made to enter at an inclination angle of 0.5 degrees after being collimated by the integrated collimating lens, the distance between the two reflector-micro-nano lens integrated elements 001 is 3cm, and therefore after 100 times of reflection, transmitted light passing through an optical path of about 3 meters is focused on the detector 402 through the other lens, and the problem of high-precision optical packaging is solved. Electrical interconnections are also integrated on transparent substrate 101 to provide electrical interconnections for powering and controlling tunable laser 401 and detector 402. The air vent 203 can be filled with suspended particles and specific gas molecular filtering materials, so that the cleanness of the chamber and the elimination of specific interference gas are ensured. Through the frequency sweeping of the tunable laser 401, high-sensitivity gas molecule detection is realized according to the TDLAS method. By using the method, the near infrared band CH can be realized4，NH3，H2And S, detecting gases such as nitrogen oxides and the like.
Example 2
An integrated micro gas absorption cell is shown in fig. 3(a), a top plate 002/bottom plate 004 structure is shown in fig. 2, and a reflector-micro nano lens integrated element is shown in fig. 1. The difference from the embodiment 1 is that the light source and the detector are large equipment equipped with a large gas spectrum analyzer which is commonly used at present and are separated from the gas absorption cell.
As shown in fig. 1, a reflector 102 and a super-surface lens 103 are prepared on one surface of a transparent substrate 101, and an antireflection film 104 is prepared on the other surface to form a reflector-micro-nano lens integrated element of a gas absorption cell. The transparent substrate 101 is made of a hard material which does not cause material absorption loss to laser used for gas sensing; the mirror 102 may be composed of a multi-layer high reflectivity film system or High Contrast Grating (HCG) mirror, with reflectivity > 99% for the laser light used for sensing; the super-surface lens 103 is a lens formed by generating a periodic micro-nano structure by micro-nano processing, and can realize the functions of collimation, focusing and the like of light beams in the sub-wavelength thickness; the antireflection film 104 is a film system composed of thin films having alternate refractive indexes, and can improve the transmittance of laser light used for sensing.
The overall structure and the working principle of the assembled gas absorption cell are shown in fig. 3(a) and 3(B), two reflector-micro-nano lens integrated elements 001 are installed between a top plate 002 and a bottom plate 004 of the gas absorption cell, and the top plate 002 and the bottom plate 004 have the same structure, which is specifically shown in fig. 2. Two reflector-micro-nano lens integrated elements 001 are respectively fixed by reflector limiting clamping grooves 202-1 of a top plate 002 and a bottom plate 004, so that reflectors 102 of the two reflector-micro-nano lens integrated elements are opposite and vertical in parallel, and two super-surface lenses 103 are staggered with each other. And a sealing plate limiting clamping groove 202-2 is arranged on the top plate 002 and the bottom plate 004 and is used for fixing two sealing plates 003 of the gas absorption cell. In fig. 2, the reflector limiting clamping groove 202-1 and the sealing plate limiting clamping groove 202-2 are grooves which are not opened, and the vent hole 203 is a through hole which opens the top plate 002/bottom plate 004 and is used for the inlet and outlet of gas.
After the gas absorption tank is assembled, gaps among all the parts are sealed and packaged by using sealant. Fig. 3(B) is a cross-section taken along a-a in fig. 3(a), and illustrates the operation of the device in a cross-sectional configuration. When the gas absorption cell is used for detection, gas is filled in the absorption cell through the vent holes 203 on the absorption cell, one beam of light is emitted from the light source 301, passes through the antireflection film 104 and the transparent substrate 101 of the one-side reflector-micro-nano lens integrated element, is collimated by the super-surface lens 103, is incident into the absorption cell at a very small inclination angle theta not greater than 1 degree, is reflected back and forth for hundreds of times between two opposite reflectors 102, is finally received by the other super-surface lens 103, passes through the transparent substrate 101 and the antireflection film 104, is emitted out of the gas absorption cell, and is received by the light detection device 302. The light source 301 may be a tunable laser or a broad spectrum light source, and the light detection device 302 may be a detector or a spectrometer.
Example 3
The difference from the absorption cell structure in embodiment 2 is that two integrated mirror-micro-nano lens elements adopt an asymmetric combined structure, the overall structure is shown in fig. 5(a), fig. 5(B) is a schematic diagram of a transmission process of light in the gas absorption cell shown in fig. 5(a) (the cross section is cut along the section C-C in fig. 5(a), and the operation principle of the device is shown in the cross-sectional structure). The micro-nano lens is used for light incidence and light emergence, the micro-nano lens is arranged at two ends of one integrated element, and reflectors are prepared on the two elements (except the position where the micro-nano lens is located). Laser enters the gas absorption pool through one micro-nano lens, and is emitted out of the other micro-nano lens after being reflected for multiple times in the pool.
The above description is only a single embodiment of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and substitutions can be made without departing from the principles of the invention. For example, through the design of lens and reflector structures, the selection of materials used by elements, and the selection of lasers and detectors, the structure can conform to the design of a gas absorption cell in a visible-near-middle infrared band; for example, the number and size of the vent holes 203 of the gas absorption cell are changed, and an external refrigeration device is added.
Claims (8)
1. An integrated micro gas absorption cell is characterized by comprising a top plate, a bottom plate, two reflector-micro nano lens integrated elements and two sealing plates, wherein the two reflector-micro nano lens integrated elements and the two sealing plates are arranged between the top plate and the bottom plate;
the top plate and the bottom plate are provided with vent holes for the inlet and outlet of gas; the top plate and the bottom plate are also provided with a reflector limiting clamping groove and a sealing plate limiting clamping groove which are respectively used for fixing the reflector-micro-nano lens integrated element and the sealing plate; the top plate and the bottom plate are processed by silicon wafers, and the reflector limiting clamping groove, the sealing plate limiting clamping groove and the vent hole are all prepared by photoetching and deep silicon etching processes;
the two reflector-micro-nano lens integrated elements are composed of a transparent substrate, a micro-nano lens and a reflector which are arranged on the front surface of the transparent substrate and an antireflection film arranged on the back surface of the transparent substrate, wherein the front surface of the transparent substrate faces the inside of the absorption pool, and the back surface of the transparent substrate faces the outside of the absorption pool; the micro-nano lens is a super-surface lens; the two reflector-micro nano lens integrated elements are oppositely arranged, and the two super surface lenses are staggered with each other; the outer sides of the super-surface lenses of the two reflector-micro-nano lens integrated elements are respectively provided with an adjustable laser and a detector;
sealing the joints of all the components after the gas absorption tank is assembled;
the reflecting mirror is composed of a plurality of layers of high-reflectivity film systems or high-contrast grating reflecting mirrors, the reflectivity of the reflecting mirror to laser used for sensing detection is more than 99%, and light is reflected between two opposite reflecting mirrors repeatedly for hundreds of times.
2. The integrated micro gas absorption cell of claim 1 wherein the reflector is one of a metal reflector, a multilayer dielectric thin film reflector, a diffractive structure reflector, or a super surface material reflector.
3. The integrated micro gas absorption cell of claim 1, wherein the super surface lens is disposed at one end of the mirror-micro nano lens integrated element.
4. The integrated micro gas absorption cell according to claim 1, wherein the mirror-micro nano lens integrated element integrally prepares the lens and the mirror by a semiconductor process, so as to realize accurate alignment of the optical axis of the lens and the optical axis of the mirror.
5. The integrated micro gas absorption cell according to claim 1, wherein the transparent substrate is made of a hard material that is non-absorptive to the wavelength of the probing laser used, and the transparent substrate has integrated electrical interconnection lines for providing electrical interconnection for powering and controlling the tunable laser and the probe.
6. The integrated micro gas absorption cell according to claim 1, wherein the vent holes are filled with a filtering or enriching material for suspending particulate matter and specific gas molecules, so as to ensure the cleanness of the absorption cell chamber and the elimination of specific interfering gases.
7. The integrated micro gas absorption cell according to claim 1, wherein the top plate further comprises a tunable laser slot and a detector slot for fixing the tunable laser and the detector, respectively.
8. An integrated micro gas absorption cell, characterized in that the structure of the absorption cell is different from the absorption cell of claim 1 in that, in the two mirror-micro-nano lens integrated elements:
one reflector-micro-nano lens integrated element consists of a transparent substrate, a reflector arranged on the front surface of the transparent substrate and an antireflection film arranged on the back surface of the transparent substrate;
the other reflector-micro-nano lens integrated element consists of a transparent substrate, micro-nano lenses and reflectors which are arranged on the front surface of the transparent substrate, and an antireflection film arranged on the back surface of the transparent substrate, wherein the number of the micro-nano lenses arranged on the front surface of the transparent substrate is two, and the two micro-nano lenses are respectively arranged at two ends of the transparent substrate.
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| JP2000111474A (en) * | 1998-10-07 | 2000-04-21 | Mitsubishi Electric Corp | High sensitivity atr analysis method and optical prism therefor |
| CN102297839B (en) * | 2011-05-20 | 2013-06-05 | 中国科学院电工研究所 | Gas absorption tank used in absorption spectrum determination |
| CN103837489A (en) * | 2012-11-26 | 2014-06-04 | 江苏远望仪器有限公司 | High-sensitivity multi-reflection optical absorbing device |
| CN103398950B (en) * | 2013-08-20 | 2015-08-19 | 天津亿利科能源科技发展股份有限公司 | A kind of Array-type multi-optical-path system for gas phase monitoring |
| CN105607166A (en) * | 2014-11-25 | 2016-05-25 | 苏州谱道光电科技有限公司 | Multiple-reflection optical sample analysis system |
| CN106353277B (en) * | 2016-08-29 | 2020-07-14 | 吉林大学 | Gas absorption cell based on copper scandium oxygen infrared transparent conducting film |
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