CN114755188A - All-fiber probe for dissolved gas in-situ detection without liquid-gas separation - Google Patents
All-fiber probe for dissolved gas in-situ detection without liquid-gas separation Download PDFInfo
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- CN114755188A CN114755188A CN202210542059.8A CN202210542059A CN114755188A CN 114755188 A CN114755188 A CN 114755188A CN 202210542059 A CN202210542059 A CN 202210542059A CN 114755188 A CN114755188 A CN 114755188A
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- 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
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/255—Splicing of light guides, e.g. by fusion or bonding
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses an all-fiber probe for dissolved gas in-situ detection without liquid-gas separation, which consists of a single-mode fiber and a hollow photonic crystal fiber, wherein a central core area is filled with liquid to be detected. The hollow photonic crystal fiber is uniformly processed with micron-sized surface micro-channels along the axial direction, and liquid to be measured dissolved with gas can enter and exit the central core area of the hollow photonic crystal fiber and the cladding air holes penetrated by the surface micro-channels through the surface micro-channels. Two ends of the hollow photonic crystal fiber are aligned with the single-mode fiber in a four-dimensional calibration mode, the hollow photonic crystal fiber and the single-mode fiber are welded by using an optical fiber welding machine, and liquid to be measured is limited to enter all cladding air holes from the end face of the hollow photonic crystal fiber. The dissolved gas in-situ detection probe designed by the invention can be arranged in liquid to be detected, can be used as a cavity for interaction of laser and dissolved gas in the liquid to be detected, and can be used for optical direct detection of the dissolved gas in the liquid to be detected without liquid-gas separation.
Description
Technical Field
The invention belongs to the technical field of optical sensing systems, and particularly relates to an all-fiber probe for dissolved gas in-situ detection without liquid-gas separation.
Background
In strong electromagnetic interference environment, in-situ detection of dissolved gas in liquid has important significance in the fields of manufacturing industry, aerospace and energy. For example, measurement of dissolved gases in electrochemical synthesis, quantification of gases in plasma-assisted combustion and catalysis, and monitoring of flammable gases in lithium ion battery electrolytes, etc., are critical to optimizing technical routes and providing safety management.
The gas detection techniques commonly used at present are chromatography, mass spectrometry and semiconductor sensing techniques. The chromatography firstly needs to sample a liquid sample to be detected and then carry out liquid-gas separation (usually takes tens of hours), and then detects gas, so that the direct detection of the dissolved gas in the liquid cannot be realized. The mass spectrometry method can not be applied to dissolved gas detection in the strong electromagnetic interference environment because strong electromagnetic interference will seriously affect the acquisition of mass spectrometry signals. The semiconductor sensing technology is also extremely easy to be interfered by strong electromagnetism, greatly influenced by humidity, short in service life and not beneficial to in-situ detection of dissolved gas in liquid.
In recent years, with the cross development among various disciplines, the optical method has the advantages of good insulation, strong electromagnetic interference resistance, high response speed and the like, so that the optical method becomes a research hotspot. Common optical gas detection methods include laser absorption spectroscopy, laser emission spectroscopy, raman scattering, faraday rotation spectroscopy, cavity ring-down spectroscopy, and the like. However, the existing optical gas detection technology is mainly developed in a gas phase environment, and the existing liquid-gas separation means is also required to be relied on to separate the dissolved gas from the liquid before the detection of the dissolved gas in the liquid is developed. The existing liquid-gas separation technology has large degassing dispersity, so that the monitoring result has large dispersity, and the content of dissolved gas is difficult to accurately evaluate; and the degassing consumes long time, which greatly restricts the real-time monitoring.
If the laser emitted by the laser is directly incident into the liquid sample to be detected for dissolved gas optical detection, the incident laser needs to be focused to the micron order by the optical lens, and the spatial size of the liquid sample to be detected is generally far larger than the beam radius. The light intensity of the laser is obviously attenuated in the process of propagation in the liquid, because the light beam inevitably diverges to the periphery in the process of propagation in the liquid sample, most of the laser is not propagated along the incident direction of the laser any more, and the light intensity of the laser is greatly reduced along the propagation direction, so that the optical detection of the dissolved gas with small concentration in the liquid phase environment cannot be carried out.
In summary, in view of the above disadvantages, it is important to provide an all-fiber probe capable of effectively restricting the radius of the laser beam for in-situ detection of the dissolved gas.
Disclosure of Invention
The invention aims to provide an all-fiber probe for in-situ detection of dissolved gas without liquid-gas separation, which is characterized by comprising a single-mode fiber and a hollow photonic crystal fiber, wherein the central core area of the hollow photonic crystal fiber is filled with liquid to be detected, and laser can be transmitted in the central core area of the hollow photonic crystal fiber at low loss and is fully contacted with the dissolved gas in the liquid to be detected. Two ends of the hollow photonic crystal fiber are connected with the single-mode fiber with the diameter close to that of the hollow photonic crystal fiber in a melting way to form a low-loss laser transmission path; uniformly processing surface micro-channels which are deep to the central core area of the hollow photonic crystal fiber on the surface of the hollow photonic crystal fiber along the axial direction; the all-fiber probe is arranged in the liquid to be detected, the liquid to be detected enters the central core area of the hollow photonic crystal fiber through the surface micro-channel, and the laser can be transmitted in the liquid to be detected in the central core area of the hollow photonic crystal fiber in a low-loss mode and fully contacts with dissolved gas in the liquid to be detected.
Preferably, the central wavelength of the hollow photonic crystal fiber is 1550nm, the working waveband range is not less than 1490-1680 nm, and the mode field diameter is not more than 10 μm, so that the near-infrared sensing requirement of the all-fiber probe is met.
Preferably, the hollow photonic crystal fiber has good insulation, electromagnetic interference resistance, pressure resistance, corrosion resistance and high temperature resistance, and the high temperature resistance is not lower than 150 ℃, so that the all-fiber probe can be arranged in the liquid to be detected.
Preferably, the length of the hollow photonic crystal fiber is not less than 0.8m, so as to ensure a sufficient absorption optical path of the laser in the all-fiber probe.
Preferably, the hollow photonic crystal fiber and the single-mode fiber are butted in a fusion welding mode, the X-Y-Z axis direction, the horizontal rotation angle and the vertical elevation angle between the end faces of the hollow photonic crystal fiber and the single-mode fiber are calibrated before fusion welding, the optical connection loss of the all-fiber probe at the 1550nm wavelength position after fusion welding is not more than 4dB, and the bread layer air hole at the end face of the hollow photonic crystal fiber is fused and sealed to ensure the optical transmission performance of the all-fiber probe.
Preferably, the surface micro-channel of the hollow photonic crystal fiber is processed by adopting a focused ion beam technology, and the surface micro-channel is deep to the central core area of the hollow photonic crystal fiber to form a continuous liquid exchange channel to be detected, so as to ensure the exchange requirement of the liquid to be detected inside and outside the central core area of the hollow photonic crystal fiber.
Preferably, the micro-channels on the surface of the hollow photonic crystal fiber are arranged on the surface of the hollow photonic crystal fiber at equal intervals, and the distance between the micro-channels on two adjacent surfaces on the surface of the hollow photonic crystal fiber is not less than 5cm and not more than 20cm, so as to ensure the mechanical strength of the all-fiber probe and the exchange speed of the liquid to be detected inside and outside the central core area of the hollow photonic crystal fiber.
Preferably, the size of the surface micro-channel of the hollow photonic crystal fiber is not more than 3 μm, and the average loss of a single surface micro-channel is not higher than 0.15dB, so as to ensure the optical transmission performance of the all-fiber probe.
When laser is transmitted in the hollow photonic crystal fiber with the central core area filled with liquid to be detected, the radius of a laser beam is always limited to the micrometer magnitude, and the size of the radius of the laser beam is not more than 5 micrometers.
Compared with the prior art, the invention has the beneficial effects that: the all-fiber probe for in-situ detection of the dissolved gas without liquid-gas separation overcomes the defects that the existing optical dissolved gas detection technology depends on the liquid-gas separation technology excessively, the laser beam divergence is serious, direct optical detection in a liquid phase cannot be realized, the in-situ detection of the dissolved gas is inconvenient, and the like, and meets the special requirements of the in-situ detection of the dissolved gas. Specifically, in the invention, the hollow photonic crystal fiber can be directly placed in liquid to be detected, and the liquid to be detected with dissolved gas can conveniently enter and exit the central core area of the hollow photonic crystal fiber, so that the hollow photonic crystal fiber provides a low-loss transmission path for light in the liquid to be detected, the beam radius is always limited to the micrometer level, and the hollow photonic crystal fiber can be fully contacted with the dissolved gas in the liquid to be detected in the central core area of the hollow photonic crystal fiber; the hollow photonic crystal fiber is also used as a place for carrying out the spectrum absorption process of the dissolved gas, can provide a long absorption optical path, greatly reduces the volume of a spectrum absorption chamber, can effectively shorten the detection period of the dissolved gas, and is convenient for realizing the in-situ detection of the dissolved gas.
Drawings
Fig. 1 is a schematic structural diagram of an all-fiber probe for in-situ detection of dissolved gas.
FIG. 2 is a schematic diagram of fusion splicing of a hollow photonic crystal fiber and a single-mode fiber.
FIG. 3 is a schematic diagram of a surface microchannel of a hollow photonic crystal fiber.
FIG. 4 is a schematic diagram of a cross-sectional partial structure of a hollow photonic crystal fiber with a micro-channel on the surface and embedded in a liquid to be measured.
Detailed Description
The invention provides an all-fiber probe for dissolved gas in-situ detection without liquid-gas separation, which consists of a single-mode fiber and a hollow photonic crystal fiber, wherein the central core area of the hollow photonic crystal fiber is filled with liquid to be detected. The all-fiber probe takes the hollow photonic crystal fiber as a core element, overcomes the defects that liquid-gas separation is required before the detection of the existing optical dissolved gas detection technology, laser beams are seriously dispersed in liquid, the volume of an optical absorption chamber is large and the like, and can be arranged in the liquid to be detected. The overall design and key elements of the all-fiber probe are described in detail below.
The whole structure schematic diagram of the all-fiber probe for the dissolved gas in-situ detection based on the hollow photonic crystal fiber and the single-mode fiber is shown in fig. 1. The two ends of the hollow photonic crystal fiber and the single-mode fiber with the diameter close to that of the hollow photonic crystal fiber are fused and connected through an optical fiber fusion splicer (as shown in figure 2), so that a low-loss laser transmission path is formed, and the connection loss is not higher than 4 dB; uniformly processing a surface micro-channel (shown in figure 3) which is deep to the central core area of the hollow photonic crystal fiber on the surface of the hollow photonic crystal fiber along the axial direction by utilizing a focused ion beam technology, wherein the size of the surface micro-channel is not more than 3 mu m, and the introduced transmission loss of a single surface micro-channel is not more than 0.15 dB; the hollow photonic crystal fiber processed with the surface micro-channel is arranged in liquid to be detected, the liquid to be detected enters a central core area of the hollow photonic crystal fiber through the surface micro-channel (as shown in figure 4) to form an all-fiber probe for dissolved gas in-situ detection, and the radius of a laser beam in the all-fiber probe is not more than 5 microns.
Referring to fig. 1, the all-fiber probe for dissolved gas in-situ detection is mainly composed of three units: the hollow photonic crystal fiber is directly arranged in the liquid to be detected, provides a path for low-loss transmission of laser in the liquid to be detected, and also provides a place for spectral absorption of dissolved gas; and the single mode fiber is connected with two ends of the hollow photonic crystal fiber, and the diameter of the single mode fiber is approximately the same as that of the hollow photonic crystal fiber. In order to meet the requirement of sufficient absorption optical path, the length of the hollow photonic crystal fiber in the all-fiber probe is not less than 0.8 m.
Referring to fig. 2, the two ends of the hollow photonic crystal fiber are fusion-connected with the single-mode fiber through a fiber fusion splicer. In the fusion process, the adjustment of the X-Y-Z axis direction, the horizontal rotation angle and the vertical elevation angle between the single-mode fiber and the hollow photonic crystal fiber is realized by adopting a four-dimensional alignment technology, the low-loss butt joint between the single-mode fiber and the hollow photonic crystal fiber is realized by regulating and controlling fusion current and fusion time, and the integral connection loss is not higher than 4 dB. In the welding process, the air holes of the bread layer at the end of the hollow photonic crystal fiber are melted and sealed, and the liquid to be measured cannot enter or exit the central core area of the hollow photonic crystal fiber from the end surface of the hollow photonic crystal fiber.
Referring to fig. 3, considering the need of liquid exchange inside and outside the central core area of the hollow photonic crystal fiber, a Focused Ion Beam (FIB) processing technique is used to process the surface micro-channel on the surface of the hollow photonic crystal fiber, which is deep to the central core area of the hollow photonic crystal fiber. Before FIB processing, firstly removing acrylic polyester coating layer at micro-channel processing point on surface of hollow photonic crystal fiber, then fixing hollow photonic crystal fiber on silicon plate adhered with conductive carbon tape, and processing pointWhere a layer of gold is deposited with a thickness not exceeding 1 μm. And arranging the hollow photonic crystal fiber on a three-dimensional workbench, and processing surface micro-channels at equal intervals along the axial direction of the hollow photonic crystal fiber. To reduce the transmission losses introduced by the surface microchannels, it is desirable to minimize the size of the surface microchannels. In the process, Ga is changed by adjusting the magnitude of ion beam current+Ion beam etching rate; changing Ga by adjusting magnitude of acceleration voltage+Ion beam bombardment speed. The space between two adjacent surface micro-channels on the surface of the hollow photonic crystal fiber is not less than 5cm and not more than 20cm, so that the mechanical strength of the all-fiber probe and the exchange speed of the liquid to be measured inside and outside the central core area of the hollow photonic crystal fiber are ensured. The size of each surface micro-channel is not more than 3 mu m, and the average loss of a single surface micro-channel is not more than 0.15dB, so that the optical transmission performance of the all-fiber probe is ensured.
Referring to fig. 4, for the all-fiber probe embedded in the liquid to be measured, the liquid to be measured can only enter and exit the central core area of the hollow photonic crystal fiber through the surface micro-channel of the hollow photonic crystal fiber, so that only the central core area of the hollow photonic crystal fiber and the air holes of the cladding penetrated by the surface micro-channel are filled with the liquid to be measured. Not less than 95% of laser is transmitted in the central core area of the hollow photonic crystal fiber, and only not more than 5% of laser leaks into the cladding; the radius of the laser beam is always limited to the micrometer magnitude, and the laser beam can be fully contacted with liquid to be measured in the central core area of the hollow photonic crystal fiber. The hollow photonic crystal fiber not only provides a low-loss transmission path of laser in a liquid to be detected, but also provides a long absorption optical path for spectral absorption of dissolved gas, and the volume of a spectral absorption cavity is greatly reduced.
Claims (8)
1. The all-fiber probe for in-situ detection of dissolved gas without liquid-gas separation is characterized by comprising a single-mode fiber and a hollow photonic crystal fiber, wherein a central core area of the hollow photonic crystal fiber is filled with liquid to be detected, and laser can be transmitted in the liquid to be detected in the central core area of the hollow photonic crystal fiber in a low-loss manner and fully contacts with the dissolved gas; two ends of the hollow photonic crystal fiber in the all-fiber probe are connected with the single-mode fiber with the diameter close to that of the hollow photonic crystal fiber in a melting way; uniformly processing surface micro-channels which are deep to the central core area of the hollow photonic crystal fiber on the surface of the hollow photonic crystal fiber along the axial direction; the all-fiber probe is arranged in the liquid to be detected, the liquid to be detected enters the central core area of the hollow photonic crystal fiber through the surface micro-channel, and the laser can be transmitted in the liquid to be detected in the central core area of the hollow photonic crystal fiber at low loss and fully contacts with the dissolved gas in the liquid to be detected.
2. The all-fiber probe for in-situ detection of dissolved gas without liquid-gas separation according to claim 1, wherein the hollow photonic crystal fiber has a center wavelength of 1550nm, an operating band of 1490-1680 nm and a mode field diameter of no greater than 10 μm, so as to meet the near-infrared sensing requirements of the all-fiber probe.
3. The all-fiber probe for in-situ detection of dissolved gas without liquid-gas separation according to claim 1, wherein the all-fiber probe material has good insulation, electromagnetic interference resistance, pressure resistance, corrosion resistance and high temperature resistance, and can withstand high temperature not lower than 150 ℃.
4. The all-fiber probe for dissolved gas in-situ detection without liquid-gas separation according to claim 1, wherein the hollow photonic crystal fiber is butted with the single-mode fiber by fusion splicing, the X-Y-Z axis direction, the horizontal corner and the vertical elevation angle between the end surfaces of the hollow photonic crystal fiber and the single-mode fiber are calibrated before fusion splicing, the optical transmission loss of the all-fiber probe at the position of 1550nm wavelength is not more than 4dB after fusion splicing, and the bread layer air hole at the end of the hollow photonic crystal fiber is fused and sealed to ensure the optical transmission performance of the all-fiber probe.
5. The all-fiber probe for in-situ detection of dissolved gas without liquid-gas separation according to claim 1, wherein the length of the hollow photonic crystal fiber is not less than 0.8m, the surface microchannel is processed by focused ion beam technology, and the surface microchannel extends to the hollow core region of the fiber, so as to ensure the exchange requirement of the liquid to be detected inside and outside the central core region of the hollow photonic crystal fiber.
6. The all-fiber probe for in-situ detection of dissolved gas without liquid-gas separation as claimed in claim 1, wherein the distance between two adjacent surface micro-channels is not less than 5cm and not more than 20cm, so as to ensure the mechanical strength of the all-fiber probe and the exchange speed of the liquid to be detected inside and outside the central core region of the hollow photonic crystal fiber.
7. The all-fiber probe for in-situ detection of dissolved gas without liquid-gas separation according to claim 1, wherein the size of the micro-channel on the surface of the hollow photonic crystal fiber is not more than 3 μm, and the average loss of the micro-channel on the single surface is not higher than 0.15dB, so as to ensure the light transmission performance of the all-fiber probe.
8. The all-fiber probe for in-situ detection of dissolved gas without liquid-gas separation as claimed in claim 1, wherein the size of the radius of the light beam in the central core region of the hollow photonic crystal fiber is not more than 5 μm, and the hollow photonic crystal fiber can be used as a cavity for interaction between laser and dissolved gas, and can be used for optical direct detection of dissolved gas without liquid-gas separation in liquid phase.
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| CN109781707A (en) * | 2019-03-13 | 2019-05-21 | 重庆大学 | It is a kind of based on optical fiber enhancing transformer oil in failure gas on-Line Monitor Device |
| CN208921621U (en) * | 2018-10-22 | 2019-05-31 | 中国计量大学 | A kind of fluorescent chemicals miniflow detector based on Hollow-Core Photonic Crystal Fibers |
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2022
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|---|---|---|---|---|
| CN101251624A (en) * | 2008-03-22 | 2008-08-27 | 燕山大学 | Photon crystal optical fiber fusion splicing three-dimensional alignment apparatus and method |
| CN101387608A (en) * | 2008-05-27 | 2009-03-18 | 重庆大学 | Ultralong Fabry-Parot interferent gas sensor and gas tester based on the sensor |
| CN104807805A (en) * | 2015-05-04 | 2015-07-29 | 华北电力大学 | Detection device for gas dissolved in transformer oil based on Raman spectrum |
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