CN115144337A - Micro-nano optical fiber gas sensor of palladium-doped carbon nanotube and preparation method and application thereof - Google Patents
Micro-nano optical fiber gas sensor of palladium-doped carbon nanotube and preparation method and application thereof Download PDFInfo
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- CN115144337A CN115144337A CN202210801239.3A CN202210801239A CN115144337A CN 115144337 A CN115144337 A CN 115144337A CN 202210801239 A CN202210801239 A CN 202210801239A CN 115144337 A CN115144337 A CN 115144337A
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Abstract
The invention discloses a palladium-doped carbon nanotube micro-nano optical fiber gas sensor and a preparation method and application thereof.
Description
Technical Field
The invention relates to the technical field of optical fiber sensing, in particular to a palladium-doped carbon nanotube micro-nano optical fiber gas sensor and a preparation method and application thereof.
Background
Sulfur hexafluoride (SF 6) is commonly used as a gas insulation medium inside a Gas Insulated Switchgear (GIS) because of its excellent insulation and arc extinguishing properties. However, when partial discharge or local overheating fault occurs inside the GIS, SF6 gas reacts with impurities such as micro water and micro oxygen, solid insulating materials, and the like, which are inevitably present inside the electrical equipment, to generate a certain characteristic product. The conventional detection methods such as a gas detection tube method, a chromatography-mass spectrometry method, an electrochemical sensor method, an ion mobility meter and an infrared absorption spectrometry method have the problems of low detection precision, easy aging of a chromatographic column, low gas selectivity, cross interference of absorption peaks of partially decomposed gas and the like, and cannot be applied to on-line monitoring of a GIS (gas insulated switchgear) on site.
The optical fiber sensing technology takes optical fibers as sensing devices, has natural insulating property, can be implanted into equipment, is not influenced by various electromagnetic signals, is easy to form an optical fiber sensing network, and has distributed measurement capability. An existing fiber-sensing-based SF6 decomposition component detection device, for example, "an in-situ detection device for SF6 decomposition components in GIS based on a fiber ring resonator" with publication number CN109765468A of 5.17.2019, is divided into a laser unit, an incident light fiber coupling unit, a fiber ring resonator, an emergent light fiber coupling unit, a detection laser and Rayleigh scattering light filtering unit, a spatial filtering unit and a spectrum acquisition unit.
The above-mentioned devices have the following disadvantages: optical devices such as reflectors, filters and lenses are largely used in the system, so that the instability and precision of the system are greatly increased, and the system is likely to be damaged or the equipment is difficult to transport. In order to realize online detection of SF6 decomposition components, extremely high requirements are put on the precision and the portability of the device, so that a micro-nano optical fiber meeting the requirements is required to be provided as a gas concentration sensor.
Disclosure of Invention
In view of this, the application provides a micro-nano optical fiber gas sensor of palladium-doped carbon nanotubes, a preparation method and an application thereof, and the gas detection sensitivity is high.
In order to achieve the technical purpose, the following technical scheme is adopted in the application:
in a first aspect, the application provides a palladium-doped carbon nanotube micro-nano optical fiber gas sensor, which comprises a laser, a palladium-doped carbon nanotube micro-nano optical fiber and a detector which are sequentially connected.
Preferably, the palladium-doped carbon nanotube micro-nano optical fiber comprises a micro-nano optical fiber area located in the middle and single-mode optical fiber areas located on two sides of the micro-nano optical fiber area, the micro-nano optical fiber area comprises a beam waist uniform area and conical areas located on two sides of the beam waist uniform area, and a palladium-doped carbon nanotube layer is deposited on the micro-nano optical fiber area.
In a second aspect, the application provides a method for preparing a palladium-doped carbon nanotube micro-nano optical fiber gas sensor, which comprises the following steps:
s1, obtaining a clean single mode fiber, and drawing the single mode fiber to form a semi-finished product with a micro-nano fiber area and a single mode fiber area under a heating condition;
s2, placing the micro-nano optical fiber area of the semi-finished product in a deionized water solution of palladium-doped carbon nano tubes, connecting one end of the single-mode optical fiber area with a laser, and introducing laser into the semi-finished product to deposit the palladium-doped carbon nano tubes to the surface of the micro-nano optical fiber area, so as to obtain the micro-nano optical fiber gas sensor of the palladium-doped carbon nano tubes.
Preferably, the clean single-mode optical fiber is obtained by the following method: removing the coating layer of the single-mode optical fiber by using wire stripping pliers, and then wiping the single-mode optical fiber by using alcohol-containing non-woven fabric.
Preferably, the preparation method of the palladium-doped carbon nanotube comprises the following steps:
K1. placing the carbon nano tube in a mixed solution of concentrated nitric acid and concentrated sulfuric acid, performing ultrasonic oscillation in a water bath, and performing centrifugal separation to obtain a precipitate;
K2. dispersing the precipitate in deionized water, then dripping the deionized water into electroless deposition liquid containing a palladium source, and filtering and drying to obtain a palladium-doped carbon nanotube;
preferably, the electroless deposition solution is prepared by the following steps: dissolving disodium ethylene diamine tetraacetate and palladium chloride in dilute ammonia water, stirring until the disodium ethylene diamine tetraacetate and the palladium chloride are completely dissolved, and then dripping into hydrazine hydrochloride solution to obtain the electroless deposition solution.
Preferably, the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1.
Preferably, the temperature of the water bath is 60-70 ℃.
In a third aspect, the application provides an application of a palladium-doped carbon nanotube micro-nano optical fiber gas sensor in gas quantitative detection.
Preferably, the gas is sulfur hexafluoride.
The beneficial effect of this application is as follows: the palladium-doped carbon nanotube micro-nano optical fiber gas sensor can enhance the sensitivity of quantitative detection of sulfur hexafluoride by combining the characteristics of low loss of the micro-nano optical fiber and high sensitivity and high selectivity of palladium-doped carbon nanotube film gas sensing.
Drawings
FIG. 1 is a schematic structural diagram of a palladium-doped carbon nanotube micro-nano optical fiber;
fig. 2 is a schematic structural diagram of the palladium-doped carbon nanotube prepared in example 1;
fig. 3 is a state density distribution curve of the palladium-doped carbon nanotube layer of the micro-nano optical fiber.
In the figure: 1. a micro-nano optical fiber area; 2. a single mode fiber region; 3. a waist-tightening uniform area; 4. a tapered region; 5. and a palladium-doped carbon nanotube layer.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The traditional detection method for the SF6 gas decomposition components mainly comprises an electrochemical sensing method, a gas chromatography method, a spectrum detection method and the like. In the method, the gas chromatography can obtain more accurate results only in a laboratory with relatively good environmental conditions, the manual maintenance cost is high, and the measurement accuracy deviation is large after the chromatography is polluted; the electrochemical sensing method has the problems of large cross interference, easy poisoning of the sensor and the like; although the spectrum detection method has the advantages of non-destructive samples, high sensitivity and the like, the design of the optical path in the equipment is difficult at present, so that the power equipment on-line monitoring device based on the spectrum detection method needs to be designed with a complex gas path, and the reliability of the equipment is reduced by detecting after gas is taken.
The optical fiber sensing technology takes optical fibers as sensing devices, has natural insulating property, can be implanted into equipment, is not influenced by various electromagnetic signals, is easy to form an optical fiber sensing network, and has distributed measurement capability. The patent cites a doped carbon nanotube film micro-nano optical fiber, and the carbon nanotube after noble metal doping modification is used as an optical fiber cladding structure, and the coated micro-nano optical fiber is used as a gas sensing device, so that gas sensing and measurement are realized. The micro-nano optical fiber has excellent flexibility and small optical loss, and most of light energy of the micro-nano optical fiber is transmitted in the form of evanescent waves around the surface of the optical fiber. If the carbon nanotube film is used as a cladding material of the micro-nano optical fiber, after the film adsorbs specific gas, the dielectric constant of the film is changed, the reflection coefficient and the absorption coefficient of the film are influenced, and further the change of light transmission in the micro-nano optical fiber is caused. By combining the characteristics of low loss of the micro-nano optical fiber and high sensitivity and high selectivity of gas sensing of the noble metal doped carbon nanotube film, the gas detection sensitivity is effectively improved.
Therefore, the invention is created.
The first aspect provides a palladium-doped carbon nanotube's optical fiber gas sensor that receives a little, including the laser that connects gradually, palladium-doped carbon nanotube's optical fiber, detector that receives a little, wherein palladium-doped carbon nanotube's optical fiber that receives a little is including the optical fiber district that receives a little that is located the middle part, the single mode fiber district that is located the optical fiber district both sides that receives a little, receive an optical fiber district including beam waist even area and being located the toper district of beam waist even area both sides, receive an optical fiber district deposit a little and have palladium-doped carbon nanotube layer.
In the scheme, the undoped carbon nanotube is used as an intrinsic semiconductor, wherein although two carriers exist, the intrinsic carrier concentration is low, and the conductivity is poor, but if trivalent Pd atoms are doped in the intrinsic semiconductor, when the trivalent Pd atoms form covalent bonds with carbon atoms, one valence electron is lacked, and a hole is left in the covalent bonds, so that the intrinsic semiconductor is changed into a p-type semiconductor, and the conductivity of the carbon nanotube is greatly enhanced. And after the Pd atom replaces one C atom on the surface of the carbon nano tube for doping, the structure of the system is obviously changed. Because the atomic radius of Pd is larger than that of C atoms, the Pd impurity causes the six-membered ring structure of the carbon nano tube to release repulsive force among atoms through deformation, so that Pd atoms obviously protrude out of the tube wall, and the Pd doping position is of a conical structure, so that the Pd-doped carbon nano tube keeps good structural stability in the gas adsorption process.
In a second aspect, the application provides a method for preparing a palladium-doped carbon nanotube micro-nano optical fiber gas sensor, which comprises the following steps:
s1, obtaining a clean single mode fiber, and drawing the single mode fiber to form a semi-finished product with a micro-nano fiber area and a single mode fiber area under a heating condition;
s2, placing the micro-nano optical fiber area of the semi-finished product in a deionized water solution of palladium-doped carbon nano tubes, connecting one end of the single-mode optical fiber area with a laser, and introducing laser into the semi-finished product to deposit the palladium-doped carbon nano tubes to the surface of the micro-nano optical fiber area, so as to obtain the micro-nano optical fiber gas sensor of the palladium-doped carbon nano tubes.
The clean single-mode optical fiber is obtained in the following mode: removing the coating layer of the single-mode optical fiber by using wire stripping pliers, and then wiping the single-mode optical fiber by using alcohol-containing non-woven fabric.
Specifically, the preparation method of the palladium-doped carbon nanotube comprises the following steps:
K1. placing the carbon nano tube in a mixed solution of concentrated nitric acid and concentrated sulfuric acid with the volume ratio of 1;
K2. dispersing the precipitate in deionized water, then dripping the deionized water into electroless deposition solution containing a palladium source, and filtering and drying to obtain a palladium-doped carbon nanotube;
in the scheme, the preparation steps of the electroless deposition solution are as follows: dissolving disodium ethylene diamine tetraacetate and palladium chloride in dilute ammonia water, stirring until the disodium ethylene diamine tetraacetate and the palladium chloride are completely dissolved, and then dripping into hydrazine hydrochloride solution to obtain the electroless deposition solution.
In a third aspect, the application provides an application of a palladium-doped carbon nanotube micro-nano optical fiber gas sensor in quantitative detection of gas, specifically, the gas is sulfur hexafluoride.
Example 1
A preparation method of a palladium-doped carbon nanotube micro-nano optical fiber gas sensor comprises the following steps:
taking a proper amount of concentrated nitric acid and concentrated sulfuric acid, stirring in a beaker, and cooling to room temperature after the solution is mixed, wherein the ratio of the nitric acid to the sulfuric acid is 1:3; placing 100mg of carbon nano tube in a prepared mixed acid solution, carrying out ultrasonic oscillation for 2.5h in a water bath at 60 ℃, then carrying out centrifugal separation by using a centrifugal machine, repeatedly washing black precipitate by using deionized water, filtering to obtain a black precipitate sample, placing the black precipitate sample in a drying box, drying and grinding the black precipitate sample into powder for later use;
dissolving disodium ethylene diamine tetraacetate and palladium chloride in dilute ammonia water, stirring until the disodium ethylene diamine tetraacetate and the palladium chloride are completely dissolved, then dripping hydrazine hydrochloride solution and continuously stirring to prepare electroless deposition solution, dissolving the treated carbon nanotube powder in deionized water, ultrasonically oscillating to uniformly disperse the carbon nanotube powder, then dripping the carbon nanotube powder into the electroless deposition solution, filtering and drying to obtain a palladium-doped carbon nanotube sample, wherein the sample is shown in figure 2;
removing a single-mode fiber coating layer by using wire stripping pliers, wiping and cleaning the optical fiber by using non-woven fabric dipped with alcohol, ensuring that no coating layer residue exists on the surface of the optical fiber, fixing the treated optical fiber on a fine adjustment sliding table by using a clamp, igniting an alcohol lamp, controlling an electric translation table to transversely move while using an outer flame to heat the treated optical fiber, and stretching at a proper speed to obtain a semi-finished product with a micro-nano optical fiber region and a single-mode fiber region;
dissolving a palladium-doped carbon nanotube sample in deionized water, placing a semi-finished micro-nano optical fiber area in the ionized water, connecting one end of a single-mode optical fiber area with a laser, introducing stronger laser into the semi-finished optical fiber, forming a vortex by a coating material, and finally depositing the vortex in a conical area to obtain the carbon nanotube film-doped micro-nano optical fiber gas sensor, wherein the state density distribution curve of the palladium-doped carbon nanotube layer of the micro-nano optical fiber is shown in figure 3.
Example 2
As shown in fig. 1, the palladium-doped carbon nanotube micro-nano optical fiber gas sensor comprises a laser, a palladium-doped carbon nanotube micro-nano optical fiber and a detector which are connected in sequence, wherein the palladium-doped carbon nanotube micro-nano optical fiber comprises a micro-nano optical fiber region 1 located in the middle and single-mode optical fiber regions 2 located on two sides of the micro-nano optical fiber region 1, the micro-nano optical fiber region 1 comprises a beam waist uniform region 3 and tapered regions 4 located on two sides of the beam waist uniform region 3, and a palladium-doped carbon nanotube layer 5 is deposited on the micro-nano optical fiber region 1.
In the scheme, the undoped carbon nanotube is used as an intrinsic semiconductor, wherein although two carriers exist, the intrinsic carrier concentration is low, and the conductivity is poor, but if a trivalent Pd atom is doped in the intrinsic semiconductor, when the trivalent Pd atom forms a covalent bond with a carbon atom, a hole is left in the covalent bond due to the lack of one valence electron, so that the original intrinsic semiconductor is changed into a p-type semiconductor, and the conductivity of the carbon nanotube is greatly enhanced. And after the Pd atom replaces one C atom on the surface of the carbon nano tube to be doped, the structure of the system is obviously changed. Because the atomic radius of Pd is larger than that of C atoms, the Pd impurities cause the six-membered ring structure of the carbon nano tube to release repulsive force among atoms through deformation, so that Pd atoms obviously protrude out of the tube wall and the conical structure at the Pd doping position, and the Pd-doped carbon nano tube keeps good structural stability in the gas adsorption process.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention.
Claims (10)
1. A palladium-doped carbon nanotube micro-nano optical fiber gas sensor is characterized by comprising a laser, a palladium-doped carbon nanotube micro-nano optical fiber and a detector which are sequentially connected.
2. The palladium-doped carbon nanotube micro-nano fiber gas sensor according to claim 1, wherein the palladium-doped carbon nanotube micro-nano fiber comprises a micro-nano fiber region (1) located in the middle and single-mode fiber regions (2) located on two sides of the micro-nano fiber region (1), the micro-nano fiber region (1) comprises a beam waist uniform region (3) and tapered regions (4) located on two sides of the beam waist uniform region (3), and a palladium-doped carbon nanotube layer (5) is deposited on the micro-nano fiber region (1).
3. The preparation method of the palladium-doped carbon nanotube micro-nano optical fiber gas sensor according to any one of claims 1 or 2, which is characterized by comprising the following steps:
s1, obtaining a clean single mode fiber, and drawing the single mode fiber to form a semi-finished product with a micro-nano fiber area (1) and a single mode fiber area (2) under a heating condition;
s2, placing the micro-nano optical fiber area (1) of the semi-finished product in a deionized water solution of palladium-doped carbon nano tubes, connecting one end of the single-mode optical fiber area (2) with a laser, and introducing laser into the semi-finished product to deposit the palladium-doped carbon nano tubes on the surface of the micro-nano optical fiber area (1), so as to obtain the micro-nano optical fiber gas sensor of the palladium-doped carbon nano tubes.
4. The method for preparing the palladium-doped carbon nanotube micro-nano fiber gas sensor according to claim 3, wherein the clean single-mode fiber is obtained in the following manner: removing the coating layer of the single-mode optical fiber by using wire stripping pliers, and then wiping the single-mode optical fiber by using alcohol-containing non-woven fabric.
5. The method for preparing the palladium-doped carbon nanotube micro-nano optical fiber gas sensor according to claim 3, wherein the method for preparing the palladium-doped carbon nanotube comprises the following steps:
K1. placing the carbon nano tube in a mixed solution of concentrated nitric acid and concentrated sulfuric acid, performing ultrasonic oscillation in a water bath, and performing centrifugal separation to obtain a precipitate;
K2. and dispersing the precipitate in deionized water, then dripping the deionized water into electroless deposition liquid containing a palladium source, and filtering and drying to obtain the palladium-doped carbon nanotube.
6. The method for preparing the micro-nano optical fiber gas sensor of the palladium-doped carbon nanotube according to claim 5, wherein the electroless deposition solution is prepared by the following steps: dissolving disodium ethylene diamine tetraacetate and palladium chloride in dilute ammonia water, stirring until the disodium ethylene diamine tetraacetate and the palladium chloride are completely dissolved, and then dripping into hydrazine hydrochloride solution to obtain the electroless deposition solution.
7. The method for preparing the palladium-doped carbon nanotube micro-nano optical fiber gas sensor according to claim 5, wherein the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1.
8. The method for preparing the palladium-doped carbon nanotube micro-nano optical fiber gas sensor according to claim 5, wherein the water bath temperature is 60-70 ℃.
9. An application of the micro-nano optical fiber gas sensor of palladium-doped carbon nanotubes in any one of claims 1-2 in quantitative gas detection.
10. Use according to claim 9, wherein the gas is sulphur hexafluoride.
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