CN111948261A - Gas sensitive element for on-line monitoring of power equipment fault characteristic gas and preparation method thereof - Google Patents
Gas sensitive element for on-line monitoring of power equipment fault characteristic gas and preparation method thereof Download PDFInfo
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- CN111948261A CN111948261A CN202010734913.1A CN202010734913A CN111948261A CN 111948261 A CN111948261 A CN 111948261A CN 202010734913 A CN202010734913 A CN 202010734913A CN 111948261 A CN111948261 A CN 111948261A
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- 238000012544 monitoring process Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000000919 ceramic Substances 0.000 claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 18
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 18
- 239000002105 nanoparticle Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- 239000002002 slurry Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 230000004044 response Effects 0.000 abstract description 16
- 239000007789 gas Substances 0.000 description 32
- 235000012431 wafers Nutrition 0.000 description 12
- 238000001514 detection method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000001680 brushing effect Effects 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006255 coating slurry Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/122—Circuits particularly adapted therefor, e.g. linearising circuits
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/122—Circuits particularly adapted therefor, e.g. linearising circuits
- G01N27/123—Circuits particularly adapted therefor, e.g. linearising circuits for controlling the temperature
Abstract
The invention discloses a gas sensitive element for on-line monitoring of power equipment fault characteristic gas, which is characterized in that: reduced graphene oxide loaded by palladium nanoparticles is used as a gas sensitive material, and the gas sensitive material is deposited on a ceramic sheet with an interdigital electrode by a brush coating method to form the gas sensitive element. The sensitive element pair H2Has high selectivity and response.
Description
Technical Field
The invention belongs to the technical field of gas detection of power equipment, and particularly relates to a gas sensitive element for on-line monitoring of fault characteristic gas of power equipment and a preparation method thereof.
Technical Field
Through the online monitoring of the fault characteristic gas of the power equipment, latent faults existing in the power equipment can be timely and accurately found, and the method has important significance in the aspect of guaranteeing the safe operation of the power equipment. Research has shown that the fault-characteristic gas of electrical equipment such as oil transformers is mainly H produced by cracking of hydrocarbons under discharge conditions2、CH4、C2H4And C2H2. Wherein H2Is a gas which can be generated by various discharge modes. Thus, for H2The realization of continuous detection with high selectivity and high sensitivity of low concentration has important significance for safe and stable operation of power equipment.
Among various types of gas-sensitive materials, graphene, as a two-dimensional atomic layered material, has the advantages of ultra-high specific surface area, ultra-fast electron mobility at room temperature and the like, and has a remarkable advantage of detecting gasThe electric signal noise is extremely low when the molecule is used, and the ultralow concentration detection of some active molecules can be realized. However, such sensitive materials are in the detection of H2It still appears unable to do so due to H2The adsorption capacity and the reaction activity on the surface of the graphene are low. By modifying the surface of palladium nanoparticles, palladium-on-H can be utilized2The specific adsorption and cracking capability of the graphene oxide, and the structural advantage of reducing the graphene oxide, the H pair is realized2High selectivity sensitive response.
In addition, the performance of the sensitive element is also influenced by the conditions of the preparation process, especially the thickness and uniformity of the sensitive layer. In order to further improve the pair H2The preparation of gas sensitive materials with moderate thickness and good uniformity is quite necessary for improving the performance.
Disclosure of Invention
The invention aims to solve the technical problems and provides a gas sensitive element for on-line monitoring of fault characteristic gas of power equipment and a preparation method thereof, wherein the sensitive element is used for detecting H with extremely low concentration (0.01 percent)2Has high selectivity and response.
In order to achieve the purpose, the invention designs a gas sensitive element for on-line monitoring of power equipment fault characteristic gas, reduced graphene oxide loaded with palladium nanoparticles is used as a gas sensitive material, the gas sensitive material is deposited on a ceramic sheet with interdigital electrodes by a brush coating method to form the gas sensitive element, and the interdigital electrode leads and the heating wire leads are fixed on an insulating base. When the device is used, a certain direct current voltage is applied to the two ends of the heating wire, so that the material on the surface of the interdigital electrode reaches a certain temperature. And the interdigital electrode lead is connected with a multimeter, the change of the resistance value of the multimeter is monitored, and whether H2 is generated or not is judged according to the change amplitude of the resistance value.
The sensitive element takes reduced graphene oxide loaded by palladium nanoparticles as a sensitive layer. The prepared sensitive element has a high response value to H2, and the actually detected concentration can be as low as 0.01%. The element can be used as a portable device for simply, reliably and real-timely monitoring the failure of the power equipment.
The gas sensitive material is a compound formed by palladium nanoparticles and reduced graphene oxide, the weight ratio of the palladium nanoparticles to the reduced graphene oxide in the gas sensitive material is 1: 20-1: 50, and the sensitivity of the gas sensitive material is obviously enhanced by compounding 2 materials together in the above ratio range.
The particle size range of the palladium nanoparticles is 10-50 nm, palladium particles smaller than the size range are easy to agglomerate, and no catalytic enhancement effect exists when the palladium particles are larger than the size range.
The preparation method of the gas sensitive element comprises the following steps:
step 1: the gas sensitive material is subjected to ultrasonic dispersion by using N, N-Dimethylformamide (DMF) to prepare uniform slurry, and the DMF solvent has high density and moderate polarity, and can well disperse graphene and the compound thereof to form more uniform dispersion liquid;
step 2: and (2) uniformly coating the slurry obtained in the step (1) on the surface of a ceramic wafer with the interdigital electrode by using a fine writing brush, and then baking the ceramic wafer under an infrared lamp until N, N-dimethylformamide in the slurry is completely volatilized, so that the thickness and the distribution of the film on the interdigital electrode are more uniform, and a gas sensitive material is deposited on the surface of the ceramic wafer to form a sensitive film.
Fixing the interdigital electrode lead on the surface of the ceramic chip in the step 2 on an insulating base; the heating wire on the back surface of the ceramic chip is also fixed on the insulating base through a lead, the heating wire is connected with a direct current voltage, the material on the surface of the interdigital electrode can reach a certain temperature (100-200 ℃) through adjusting the voltage, and finally, the dustproof metal cap is covered on the insulating base to cover the ceramic chip. The resistance value is 10-500 k omega when the temperature is 100-200 ℃;
the mass of the gas sensitive material is 100-500 mg, the volume of N, N-dimethylformamide used is 0.5-2 mL, and the proportion is that the material has a proper concentration in DMF so as to be completely brushed on the interdigital electrode each time, the concentration is too low, the brushing times are increased, and the time cost is increased; too high concentration and too much material can not be brushed on the interdigital electrode at one time, thereby influencing later-period repeatability.
The thickness range of the sensitive film is 50-500 mu m, the sensitive film is too thick, and gas cannot permeate into a bottom layer material and interact with the bottom layer material, so that a response signal is poor; the material is too thin and the stability of the sensitive element is not good.
When the ceramic wafer is baked under an infrared lamp, the temperature sensed by the surface of the ceramic wafer is controlled to be 150-200 ℃ so as to prevent the sensitive film from cracking.
The invention has the beneficial effects that:
1. the invention selects H pair based on the specific adsorption between the target gas and the sensitive material2The noble metal palladium nano particles with high selectivity are uniformly dispersed on the surface of the graphene sheet so as to fully play the dual functions of catalysis and adsorption;
2. in the preparation process of the sensitive element, the response value of the sensitive element to the target gas is improved by screening out the appropriate thickness of the sensitive film;
3. the sensitive element pair H screened by the invention2Has higher selectivity and response, and the preparation process method is simple and feasible.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of reduced graphene oxide supported on palladium nanoparticles;
fig. 2 is a response curve of the sensor testing 0.01% hydrogen.
Fig. 3 is a Scanning Electron Microscope (SEM) image of palladium nanoparticle-supported reduced graphene oxide;
FIG. 4 shows the response of the sensor to test 0.01% hydrogen.
Detailed Description
The invention is described in further detail below with reference to the following figures and examples:
example 1:
step 1: 100mg of the gas sensitive material was mixed with 1.5mL of N, N-dimethylformamide to prepare a slurry having good uniformity. FIG. 1 shows the surface morphology structure of a sensitive material (reduced graphene oxide supported by palladium nanoparticles);
step 2: dipping the paste of the whole pen head with a superfine writing brush, smearing the paste on the surface of a ceramic wafer inlaid with an interdigital electrode, then, placing the ceramic wafer under an infrared lamp at 160 ℃ for baking until the solvent is completely evaporated to dryness, forming a layer of sensitive film on the interdigital electrode, taking a plurality of identical ceramic wafers inlaid with the interdigital electrode, respectively brushing sensitive films with different thicknesses on the surfaces of the ceramic wafers, and baking according to the method to obtain a plurality of elements with sensitive films with different thicknesses; the sensitive element works at the temperature of 200 ℃, and the resistance value between the two interdigital electrodes is 10-100 k omega;
the response value of the sensitive element to the target gas is defined as: r ═ Sg/RaWherein R isa、RgThe resistance values of the sensitive element exposed to clean air and target gas, respectively.
H is carried out on a plurality of sensitive elements prepared in the way2Response test and thus select pair H2The sensitive element with the highest response value. Tests show that the sensitive element obtained by brushing the sensitive film for about 4 times is H2The response value is highest, the actual minimum detection limit can reach 0.01 percent, and as shown in figure 2, real-time online monitoring of the power equipment fault can be realized.
Example 2:
step 1: adding 300mg of gas sensitive material into 2mL of N, N-dimethylformamide, and fully mixing to form homogenate, wherein the structure of the used sensitive material (reduced graphene oxide loaded with palladium) is shown in FIG. 3;
step 2: dipping a pen point slurry with an ultrafine brush pen, uniformly coating the slurry on the surface of a ceramic wafer inlaid with an interdigital electrode, then placing the ceramic wafer under an infrared lamp at 200 ℃ for baking until a solvent is completely dispersed, forming a layer of sensitive film on the surface of the interdigital electrode, additionally, respectively coating slurries with different times on a plurality of identical ceramic wafers, and fully baking by the infrared lamp to obtain a plurality of sensitive elements with different sensitive film thicknesses; the sensitive element works under the heating condition of 150 ℃, and the resistance value is 100-500 k omega;
defining the response value of the sensitive element as S ═ Ra/RgWherein R isa、RgRespectively, the resistance values in clean air and the gas to be measured.
H is carried out on a plurality of sensitive elements prepared in the way2And thus optimizing the response test to H2The best responding sensing element. The sensitive material is coated on the surface of the interdigital electrode for about 7 times, and the obtained sensitive element pair H2The highest response value. H emitted from the insulation part when the power equipment starts to break down2The concentration is much higher than 0.01%, so the sensitive element is required to be capable of resisting 0.01% H2With high response, FIG. 4 shows that the element optimized by the sensitive layer can realize 0.01% H2Detection of (3).
Details not described in this specification are within the skill of the art that are well known to those skilled in the art.
Claims (8)
1. The utility model provides a gaseous sensing element towards gaseous on-line monitoring of power equipment fault signature which characterized in that: reduced graphene oxide loaded by palladium nanoparticles is used as a gas sensitive material, and the gas sensitive material is deposited on a ceramic sheet with an interdigital electrode by a brush coating method to form the gas sensitive element.
2. The gas sensor oriented to power equipment fault signature gas on-line monitoring of claim 1, wherein: the gas sensitive material is a compound formed by palladium nanoparticles and reduced graphene oxide, and the weight ratio of the palladium nanoparticles to the reduced graphene oxide in the gas sensitive material is 1: 20-1: 50.
3. The gas sensor oriented to power equipment fault signature gas on-line monitoring of claim 1, wherein: the particle size range of the palladium nanoparticles is 10-50 nm.
4. A method of making a gas sensor according to claim 1, comprising the steps of:
step 1: carrying out ultrasonic dispersion on the gas sensitive material by using N, N-dimethylformamide to prepare uniform slurry;
step 2: and (2) uniformly coating the slurry obtained in the step (1) on the surface of a ceramic wafer with interdigital electrodes, and then baking the ceramic wafer under an infrared lamp until N, N-dimethylformamide in the slurry is completely volatilized, so that a gas sensitive material can be deposited on the surface of the ceramic wafer to form a sensitive film.
5. The method for producing a gas sensor according to claim 4, wherein: fixing the interdigital electrode lead on the surface of the ceramic chip in the step 2 on an insulating base; the heating wire on the back of the ceramic chip is also fixed on the insulating base through a lead, and finally, the dustproof metal cap is covered on the insulating base to cover the ceramic chip.
6. The method for producing a gas sensor according to claim 4, wherein: the mass range of the gas sensitive material is 100-500 mg, and the volume range of the used N, N-dimethylformamide is 0.5-2 mL.
7. The method for producing a gas sensor according to claim 4, wherein: the thickness range of the sensitive film is 50-500 mu m.
8. The method for producing a gas sensor according to claim 4, wherein: when the ceramic plate is placed under an infrared lamp for baking, the temperature sensed by the surface of the ceramic plate is controlled to be 150-200 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010734913.1A CN111948261A (en) | 2020-07-27 | 2020-07-27 | Gas sensitive element for on-line monitoring of power equipment fault characteristic gas and preparation method thereof |
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| CN202010734913.1A CN111948261A (en) | 2020-07-27 | 2020-07-27 | Gas sensitive element for on-line monitoring of power equipment fault characteristic gas and preparation method thereof |
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