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CN-119375310-B - Be used for C4F7N-local fault decomposition component detection sensor and preparation method thereof

CN119375310BCN 119375310 BCN119375310 BCN 119375310BCN-119375310-B

Abstract

The invention provides a sensor for detecting a C 4 F 7 N local fault decomposition component and a preparation method thereof, belonging to the technical field of gas sensing. The sensor comprises a gas-sensitive material, a screening layer material and interdigital electrodes, wherein the gas-sensitive material covers the surfaces of the interdigital electrodes, and the screening layer material covers the surfaces of the gas-sensitive material. According to the invention, snO 2 、Pd-SnO 2 and MoS2-SnO 2 are used as gas-sensitive materials, the gas-sensitive materials are covered on the surfaces of the interdigital electrodes in a drop coating mode, and then a screening layer material Co 3 (HITP) 2 is covered on the surfaces of the gas-sensitive materials in a screen printing mode, so that a double-layer sensing structure is formed. The double-layer structure sensor can detect the decomposition component C 3 F 6 、CO、CHF 3 under the strong interference of C 4 F 7 N background gas, three gas-sensitive materials respectively have certain response selectivity to three gases, the detection lower limit is respectively 0.195 ppm, 3.12 ppm and 3.66 ppm, and the double-layer structure sensor array has certain qualitative and quantitative recognition capability to mixed gases.

Inventors

  • XIAO SONG
  • WU PENG
  • LI DAI
  • TANG JU
  • ZHANG XIAOXING

Assignees

  • 武汉大学

Dates

Publication Date
20260512
Application Date
20241023

Claims (8)

  1. 1. The sensor for detecting the C 4 F 7 N local fault decomposition component is characterized by comprising a gas-sensitive material, a screening layer material and an interdigital electrode, wherein the gas-sensitive material is covered on the surface of the interdigital electrode and is used for generating selective response with the decomposition components C 3 F 6 , CO and CHF 3 of C 4 F 7 N molecules, the screening layer material is covered on the surface of the gas-sensitive material and is used for confining the C 4 F 7 N molecules and eliminating interference of the C 4 F 7 N molecules on the decomposition components of the C3232N molecules, the screening layer material comprises Co 3 (HITP) 2 , and the gas-sensitive material comprises SnO 2 、Pd-SnO 2 、MoS 2 -SnO 2 ; The preparation method of the sensor for detecting the C 4 F 7 N partial fault decomposition component comprises the following steps: (1) Preparing SnO 2 、Pd-SnO 2 、MoS 2 -SnO 2 solutions respectively, dripping the solutions onto the surfaces of the interdigital electrodes respectively, and vacuum drying to form a gas-sensitive layer; (2) Covering the Co 3 (HITP) 2 solution on the surface of the gas-sensitive layer in a screen printing mode, and drying in vacuum to obtain the sensor for detecting the C 4 F 7 N partial fault decomposition component.
  2. 2. The sensor for detecting C 4 F 7 N local fault-resolved components according to claim 1, wherein the mass ratio of the gas sensitive material to the screening layer material is 20:1.
  3. 3. The sensor for C 4 F 7 N partial fault resolution component detection of claim 1, wherein the Co 3 (HITP) 2 is prepared by the steps of: S1, mixing Co (NO 3 ) 2 ·6H 2 O and DMF, heating to 65 ℃, and then adding 2,3,6,7,10, 11-hexaaminotrityl hexachloride solution to obtain a mixture; S2, adding NaOAc solution into the mixture, reacting at 65 ℃ for 2h, filtering, centrifugally washing for multiple times, and drying to obtain Co 3 (HITP) 2 particles.
  4. 4. A sensor for the detection of C 4 F 7 N localized trouble shooting components according to claim 3, wherein the molar ratio of Co (NO 3 ) 2 ·6H 2 O to 2,3,6,7,10, 11-hexaaminotrityl hexachloride is 1:0.25.
  5. 5. The sensor for C 4 F 7 N partial fault resolution component detection of claim 1, wherein the SnO 2 preparation step comprises: S1, uniformly mixing SnCl 2 ·2H 2 O, ethanol and DMF, then adding polyvinylpyrrolidone, and fully mixing at 60-70 ℃ to form a viscous colloid mixture as a precursor solution of electrostatic spinning; s2, carrying out electrostatic spinning on the precursor solution to obtain nanofibers; And S3, annealing the nanofiber at 500 ℃ to obtain the pure SnO 2 nanofiber.
  6. 6. The sensor for C 4 F 7 N partial fault resolution component detection of claim 1, wherein the Pd-SnO 2 preparation step comprises: s1, fully mixing SnCl 2 ·2H 2 O、C 6 H 5 Na 3 O 7 ·2H 2 O、PdCl 2 , ethanol and water to obtain a precursor suspension; S2, reacting the precursor suspension at 180 ℃ for 12 h, cooling to room temperature, filtering, centrifugally washing and drying to obtain Pd-SnO 2 particles.
  7. 7. The sensor for the detection of C 4 F 7 N partial fault resolution components of claim 6, wherein the SnCl 2 ·2H 2 O、C 6 H 5 Na 3 O 7 ·2H 2 O、PdCl 2 molar ratio is 5:10:0.2.
  8. 8. The sensor for C 4 F 7 N partial fault resolution component detection as claimed in claim 1, wherein the step of preparing MoS 2 -SnO 2 comprises: S1, uniformly mixing Na 2 MoO 4 ·2H 2 O、CH 3 CSNH 2 with water, then adding hexadecyl trimethyl ammonium bromide, and uniformly mixing to obtain a mixture; S2, reacting the mixture at 180 ℃ for 24h, cooling to room temperature, centrifuging, washing and drying to obtain MoS 2 nanoflower; S3, fully mixing MoS 2 nanoflower, snCl 2 ·2H 2 O and water, reacting at 180 ℃ for 12 h, cooling to room temperature, and repeatedly centrifuging, washing and drying to obtain MoS 2 -SnO 2 particles.

Description

Sensor for detecting C 4F7 N local fault decomposition component and preparation method thereof Technical Field The invention relates to the technical field of gas sensing, in particular to a sensor for detecting a C 4F7 N partial fault decomposition component and a preparation method thereof. Background SF 6 is an insulating gas commonly used in the power industry and has excellent insulating and arc extinguishing properties. However, at the same time, SF 6 is also a gas with strong greenhouse effect, and is limited in use by the plain text of the terms "kyoto protocol" and "paris protocol". To alleviate the dependence of power systems on SF 6, expert students in the industry are beginning to find new environmental friendly gases as insulating mediums for power systems. Wherein, C 4F7 N is used as a novel environment-friendly gas, the insulating property of the novel environment-friendly gas is 2.2 times of SF 6, the potential value of greenhouse benefit is only 1/11 of SF 6, and the novel environment-friendly gas has extremely high application potential. In the operating field, with the increase of the operating time, the gas-insulated equipment inevitably has local defects such as free metal particles, poor conductor contact and the like, which cause the occurrence of local discharge and local overheat faults. Under these faults, C 4F7 N will decompose and form stable characteristic gas by-products. By detecting C 3F6, CO, and CHF 3 in these characteristic gas byproducts, faults inside the device can be discovered in time and corresponding operation and maintenance measures can be developed. However, C 4F7 N, due to its strong electron affinity and the active functional group cyano (-CN), produces a very strong interference with the detection of its resolved components. Therefore, in the early stage of the application of the C 4F7 N insulating device, it is highly desirable to provide a gas sensor which is simple in preparation steps, low in cost, can operate at room temperature, and has high sensitivity and selectivity to breakdown components to cope with internal latent faults which may occur in the device during operation. Disclosure of Invention Aiming at the defects of the prior art, the invention provides the sensor for detecting the C 4F7 N local fault decomposition component of the environment-friendly insulating gas and the preparation method thereof, and the sensor is used for monitoring the C 4F7 N fault decomposition component in real time, can discover faults in equipment in time, and is beneficial to spreading corresponding operation and maintenance measures in time. In order to achieve the above purpose, the specific technical scheme of the invention is as follows: A sensor for detecting a C 4F7 N local fault decomposition component comprises a gas-sensitive material, a screening layer material and an interdigital electrode, wherein the gas-sensitive material is covered on the surface of the interdigital electrode, the screening layer material is covered on the surface of the gas-sensitive material, and the screening layer material comprises a two-dimensional metal organic framework material Co 3(HITP)2. Further, the gas-sensitive material is covered on the surface of the interdigital electrode in a dripping mode, and the screening layer material is covered on the surface of the gas-sensitive material in a screen printing mode. Further, the mass ratio of the gas-sensitive material to the screening layer material is 20:1. Further, the preparation steps of the Co 3(HITP)2 are as follows: S1, mixing Co (NO 3)2·6H2 O and DMF, heating to 65 ℃, and then adding aqueous solution of 2,3,6,7,10, 11-hexaaminotrityl hexahydrochloride (HATP.6HCl) to obtain a mixture; S2, adding 2 mol/L NaOAc aqueous solution into the mixture, reacting at 65 ℃ for 2h, filtering the obtained black powder, centrifugally washing for multiple times, and drying to obtain Co 3(HITP)2 particles. Still further, the molar ratio of Co (NO 3)2·6H2 O to 2,3,6,7,10, 11-hexaaminotrityl hexahydrochloride) was 1:0.25. Further, the gas sensitive material includes SnO 2 (tin dioxide), pd—sno 2 (palladium doped tin dioxide), moS 2-SnO2 (tin dioxide doped molybdenum disulfide). Further, the SnO 2 is obtained by carrying out electrostatic spinning on raw materials including tin dichloride and then calcining. Further, the preparation steps of the SnO 2 include: S1, uniformly mixing SnCl 2·2H2 O, ethanol and N, N-Dimethylformamide (DMF) at room temperature, then adding polyvinylpyrrolidone (PVP), and fully mixing at 60-70 ℃ to form a viscous colloid mixture as a precursor solution of electrostatic spinning; s2, carrying out electrostatic spinning on the precursor solution to obtain nanofibers; S3, annealing the nanofiber at 500 ℃ in air for 2 hours to remove PVP and obtain the pure SnO 2 nanofiber. Still further, the polyvinylpyrrolidone has a molecular weight of 1300000. Further, the mass ratio of the SnCl 2·2H2 O to the polyvinylpyrrolidone