CN114216936A - Preparation method and application of cubic phase molybdenum carbide nanowire gas sensor - Google Patents
Preparation method and application of cubic phase molybdenum carbide nanowire gas sensor Download PDFInfo
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- CN114216936A CN114216936A CN202111560395.7A CN202111560395A CN114216936A CN 114216936 A CN114216936 A CN 114216936A CN 202111560395 A CN202111560395 A CN 202111560395A CN 114216936 A CN114216936 A CN 114216936A
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- 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
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- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention provides a preparation method and application of a cubic phase molybdenum carbide nanowire gas sensor6The gas sensor prepared by the method can make up the SF of the sensor in the prior art6The lowest detection limit of the defects on the detection of the decomposition components is 10ppm, the sensitivity is high, and the detection can be carried out on SF at 50 DEG C6The decomposed component gas responds, and the working temperature of the conventional resistance-type gas sensor is greatly reduced.
Description
Technical Field
The invention belongs to the field of novel nano materials and the technical field of gas-sensitive sensing, and particularly relates to a preparation method and application of a cubic phase molybdenum carbide nanowire gas-sensitive sensor.
Background
SF6Gas Insulated Switchgear (GIS) is reliable in operation and maintenanceThe transformer substation has the advantages of small quantity, small actual occupied area and the like, is widely concerned by the power industry after being put into operation from the beginning, and gradually becomes a symbolic device of a modern transformer substation. However, after GIS is operated for a long time, partial heat release and partial discharge of different degrees still occur to cause SF6The decomposition of the insulating medium reacts with trace moisture and trace oxygen existing in the GIS to finally generate SO2、SO2F2SF typified by isogas6The component gas is decomposed. The content and concentration change characteristics of the component gases are closely related to the fault type of the GIS and the severity of the fault occurrence. Therefore, the characteristic component gases are effectively monitored in time, and the occurrence of insulation accidents can be effectively reduced. At present, gas detection methods mainly include a gas chromatography method, a detection tube method, an optical detection method, a nano gas sensor method and the like. The nano gas-sensitive sensor method has the advantages of low cost, convenience in production, small volume, sensitivity to characteristic gas and the like, and is a development direction of built-in sensing and online monitoring of gas insulation equipment in the future.
Based on the problems in the prior art, the invention aims to provide a preparation method of a cubic phase molybdenum carbide nanowire gas sensor, and the preparation method is applied to SF in Gas Insulated Switchgear (GIS)6The invention discloses a method for detecting decomposition components, which aims to prepare an electrode sensing module by using cubic phase molybdenum carbide nanowires and construct a gas sensor to realize SF (sulfur hexafluoride) detection6Detecting the decomposed component gas; the gas sensor can compensate the SF of the sensor in the prior art6The lowest detection limit of the defects on the detection of the decomposition components is 10ppm, the sensitivity is high, and the detection can be carried out on SF at 50 DEG C6The decomposed component gas responds, and the working temperature of the conventional resistance-type gas sensor is greatly reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the technical scheme adopted by the invention for solving the problems in the prior art is as follows:
a preparation method of a cubic phase molybdenum carbide nanowire gas sensor is characterized by comprising the following steps:
step one, preparing a cubic phase molybdenum carbide nanowire: dissolving a certain amount of ammonium heptamolybdate and aniline in deionized water, dropwise adding a certain molar mass of aqueous hydrogen chloride solution under magnetic stirring, placing the mixed solution in an oil bath at 30-80 ℃ for reaction for 4-6 hours, filtering and cleaning the precipitate to obtain a preliminary Mo precursor, grinding the precursor, and carbonizing at the temperature of 500-700 ℃ in a reducing atmosphere to obtain a cubic phase molybdenum carbide nanowire;
and secondly, ultrasonically washing a platinum interdigital electrode arranged in the gas sensor by using deionized water, dispersing the cubic-phase molybdenum carbide nanowire obtained in the first step in an ethylene glycol solution, ultrasonically dispersing for 30-50 minutes in an ultrasonic cleaner at normal temperature to obtain a molybdenum carbide nanowire-ethylene glycol mixed solution, coating the mixed solution on the cleanly washed interdigital electrode by using a screen printing technology, putting the platinum interdigital electrode coated with the cubic-phase molybdenum carbide nanowire-ethylene glycol mixed solution into a vacuum oven, drying for 8-12 hours at the temperature of 60-100 ℃ in vacuum until the ethylene glycol is completely volatilized, forming a stable molybdenum carbide film to cover an interdigital electrode sensing area, and obtaining the cubic-phase molybdenum carbide nanowire gas sensor.
In the first step, 1.24-4.15g of ammonium heptamolybdate and aniline are dissolved in 10-30mL of deionized water, 1mol/L of aqueous hydrogen chloride solution is dropwise added under magnetic stirring, and the pH value is adjusted to 4-5 to obtain a mixed solution.
And in the first step, the mixed solution is placed in an oil bath at the temperature of 30-80 ℃ for reaction for 4-6 hours, and the precipitate is filtered and cleaned to obtain a primary Mo precursor.
The application of the cubic phase molybdenum carbide nanowire gas sensor is characterized in that the cubic phase molybdenum carbide nanowire gas sensor is applied to detection of SF6The method comprises the following specific steps of:
step 1, parameter setting: setting the working temperature of the cubic phase molybdenum carbide nanowire to be normal temperature (25 ℃) to 350 ℃, wherein the gas concentration is 10ppm to 300 ppm;
step 2, gas-sensitive testing: loading the cubic phase molybdenum carbide nanowire gas sensor into a testing device, and introducing inert gas helium into the testing device until the initial resistance value of molybdenum carbide is stable and is recorded as R0Then, immediatelyThe gas to be measured is introduced, and the resistance value after the resistance is stabilized is recorded as R1And calculating the relative variation of the resistance of the sensor (namely the gas-sensitive response value): r ═ S0/R1And the response capability of the cubic phase molybdenum carbide nanowire gas sensor to gas to be measured is reflected by the size of the sensor.
Compared with the prior art, the cubic phase molybdenum carbide nanowire gas sensor has the following advantages: cubic phase molybdenum carbide Mo obtained at 500 ℃ carbonization temperature2C-500 as an example, at 50 ℃ to SO2The gas sensitive response of the gas sensor reaches 1.16 at the lowest, and the gas sensor is used for SO2F2The gas-sensitive response of the gas sensor can reach 1.12, and Mo is generated along with the increase of the working temperature and the gas concentration2C to SO2、SO2F2The gas-sensitive response of the nano-wire is larger and larger, the highest gas-sensitive response can reach 3.17 and 3.61 respectively, and the prepared cubic phase molybdenum carbide nano-wire is used for SF6The decomposition component detection material not only shows excellent gas-sensitive adsorption capacity, but also has excellent detection temperature.
Drawings
FIG. 1: in example 1 of the present invention, Mo is present at different detection temperatures2C-500 as gas-sensitive detection material for SO with different concentrations2A gas sensitive response graph of (a);
FIG. 2: in example 2 of the present invention, Mo is present at different detection temperatures2C-600 as gas-sensitive detection material for SO with different concentrations2A gas sensitive response graph of (a);
FIG. 3: in example 3 of the present invention, Mo is present at different detection temperatures2C-700 as gas-sensitive detection material for SO with different concentrations2A gas sensitive response graph of (a);
FIG. 4: in example 4 of the present invention, Mo is present at different detection temperatures2C-500 as gas-sensitive detection material for SO with different concentrations2F2A gas sensitive response graph of (a);
FIG. 5: in example 5 of the present invention, Mo is present at different detection temperatures2C-600 as gas-sensitive detection material for SO with different concentrations2F2A gas sensitive response graph of (a);
FIG. 6: in example 6 of the present invention, Mo is added at different detection temperatures2C-700 as gas-sensitive detection material for SO with different concentrations2F2A gas sensitive response graph of (a);
FIG. 7: three kinds of Mo at different temperatures2C sample for different concentrations of SO2A gas sensitive response graph;
FIG. 8: three kinds of Mo at different temperatures2C sample for different concentrations of SO2F2Gas sensitive response graph.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments and the accompanying drawings.
Example 1
Dissolving 1.24-4.15g of ammonium heptamolybdate and aniline in 10-30mL of deionized water, dropwise adding 1mol/L aqueous solution of hydrogen chloride under magnetic stirring, adjusting the pH value to 4-5, placing the mixed solution in an oil bath at 30-80 ℃ for reaction for more than 4-6 hours, filtering and cleaning the obtained precipitate to obtain a Mo precursor preliminarily, grinding the precursor, and carbonizing at 500 ℃ for 1-3 hours in a reducing atmosphere to obtain Mo2Samples of C-500. Mo obtained in the example2Dispersing C-500 nanowires in an ethylene glycol solution, performing ultrasonic dispersion for 30-50 minutes in an ultrasonic cleaner at normal temperature to obtain a molybdenum carbide nanowire-ethylene glycol mixed solution, coating the mixed solution on a rinsed interdigital electrode by a silk screen printing technology, putting the platinum interdigital electrode coated with the cubic phase molybdenum carbide nanowire-ethylene glycol mixed solution into a vacuum oven, drying for 8-12 hours at the temperature of 60-100 ℃ in vacuum until ethylene glycol is completely volatilized, forming a stable molybdenum carbide film to cover an interdigital electrode sensing area, and obtaining Mo2C-500 gas sensor.
Mo obtained in the example2The C-500 nanowire gas sensor is arranged in the detection device and is used for detecting SO under the conditions of different temperatures and different concentrations2Performing gas-sensitive detection, the sensor response curve is shown in FIG. 1, and under normal temperature, different SO2The concentration and the response value are all floated at about 1; SO at the same detection temperature except at normal temperature2The higher the gas concentration, the larger the response value; at the same concentration, the response is basically shown along with the increase of the temperatureAnd (4) an upward trend. Wherein, at 50 ℃, 30ppm of SO can be successfully detected at the lowest2The response value was 1.6, and at 350 ℃ the lowest successful detection of 10ppm SO was obtained2The response value was 1.12.
Example 2
Dissolving 1.24-4.15g of ammonium heptamolybdate and aniline in 10-30mL of deionized water, dropwise adding 1mol/L aqueous solution of hydrogen chloride under magnetic stirring, adjusting the pH value to 4-5, placing the mixed solution in an oil bath at 30-80 ℃ for reaction for more than 4-6 hours, filtering and cleaning the obtained precipitate to obtain a Mo precursor preliminarily, grinding the precursor, and carbonizing the precursor at 600 ℃ for 1-3 hours under a reducing atmosphere to obtain Mo2Sample C-600. Mo obtained in the example2Dispersing C-600 nanowires in an ethylene glycol solution, performing ultrasonic dispersion for 30-50 minutes in an ultrasonic cleaner at normal temperature to obtain a molybdenum carbide nanowire-ethylene glycol mixed solution, coating the mixed solution on a rinsed interdigital electrode by a silk screen printing technology, putting the platinum interdigital electrode coated with the cubic phase molybdenum carbide nanowire-ethylene glycol mixed solution into a vacuum oven, drying for 8-12 hours at the temperature of 60-100 ℃ in vacuum until ethylene glycol is completely volatilized, forming a stable molybdenum carbide film to cover an interdigital electrode sensing area, and obtaining Mo2C-600 gas sensor.
Mo obtained in the example2The C-600 nanowire gas sensor is arranged in the detection device and is used for detecting SO under the conditions of different temperatures and different concentrations2The gas-sensitive detection is carried out, the response curve of the sensor is shown in figure 2, and different SOs are detected under the normal temperature state2The concentration and the response value are all floated around 1. Outside the normal temperature state, at the same detection temperature, SO2The higher the gas concentration, the larger the response value. At the same concentration, the response basically increases with the increase of the temperature. Wherein 30ppm SO was detected at 350 deg.C2Response was 1.14, with a minimum of 100ppm SO successfully detected at 50 deg.C2The response is 1.1.
Example 3
Dissolving 1.24-4.15g of ammonium heptamolybdate and aniline in 10-30mL of deionized water, and dropwise adding 1mol/L of hydrogen chloride water under magnetic stirringAdjusting the pH value of the solution to 4-5, placing the mixed solution in an oil bath at the temperature of 30-80 ℃ for reaction for more than 4-6 hours, filtering and cleaning the obtained precipitate to obtain a precursor of Mo preliminarily, grinding the precursor, and carbonizing the precursor at the temperature of 700 ℃ for 1-3 hours in a reducing atmosphere to obtain the Mo2Sample of C-700. Mo obtained in the example2Dispersing C-700 nanowires in an ethylene glycol solution, performing ultrasonic dispersion for 30-50 minutes in an ultrasonic cleaner at normal temperature to obtain a molybdenum carbide nanowire-ethylene glycol mixed solution, coating the mixed solution on a rinsed interdigital electrode by a silk screen printing technology, putting the platinum interdigital electrode coated with the cubic phase molybdenum carbide nanowire-ethylene glycol mixed solution into a vacuum oven, drying for 8-12 hours at the temperature of 60-100 ℃ in vacuum until ethylene glycol is completely volatilized, forming a stable molybdenum carbide film to cover an interdigital electrode sensing area, and obtaining Mo2C-700 gas sensor.
Mo obtained in the example2The C-700 nanowire gas sensor is arranged in the detection device and is used for detecting SO under the conditions of different temperatures and different concentrations2The gas-sensitive detection is carried out, the response curve of the sensor is shown in figure 3, and different SOs are detected under the normal temperature state2The concentration and the response value are all floated around 1. Outside the normal temperature state, at the same detection temperature, SO2The higher the gas concentration, the larger the response value. At the same concentration, the response basically increases with the increase of the temperature. Wherein, at 350 ℃, the lowest successful detection of 100ppm SO can be realized2Response was 1.14, with a minimum of only 300ppm SO successfully detected at 50 deg.C2The response is 1.11.
Example 4
Dissolving 1.24-4.15g of ammonium heptamolybdate and aniline in 10-30mL of deionized water, dropwise adding 1mol/L aqueous solution of hydrogen chloride under magnetic stirring, adjusting the pH value to 4-5, placing the mixed solution in an oil bath at 30-80 ℃ for reaction for more than 4-6 hours, filtering and cleaning the obtained precipitate to obtain a Mo precursor preliminarily, grinding the precursor, and carbonizing at 500 ℃ for 1-3 hours in a reducing atmosphere to obtain Mo2Samples of C-500. Mo obtained in the example2The C-500 nanowires are dispersed in a glycol solution, often in an ultrasonic cleanerUltrasonically dispersing for 30-50 minutes at a warm state to obtain a molybdenum carbide nanowire-ethylene glycol mixed solution, coating the mixed solution on a cleaned interdigital electrode by a silk screen printing technology, putting the platinum interdigital electrode coated with the cubic phase molybdenum carbide nanowire-ethylene glycol mixed solution into a vacuum oven, drying for 8-12 hours at the temperature of 60-100 ℃ in vacuum until ethylene glycol is completely volatilized, forming a stable molybdenum carbide film to cover a sensing area of the interdigital electrode, and thus obtaining Mo2C-500 gas sensor.
Mo obtained in the example2The C-500 nanowire gas sensor is arranged in the detection device and is used for detecting SO at different temperatures and different concentrations2F2The gas-sensitive detection is carried out, the response curve of the sensor is shown in figure 4, and different SOs are detected under the normal temperature state2F2The concentration and the response value are all floated at about 1; SO at the same detection temperature except at normal temperature2F2The higher the gas concentration, the larger the response value; at the same concentration, the response tends to increase with the increase of the temperature. Wherein at 50 ℃, the lowest successful detection of 50ppm SO is achieved2F2The response value was 1.12, and 30ppm SO was detected at 350 ℃ with minimum success2F2The response value was 1.21.
Example 5
Dissolving 1.24-4.15g of ammonium heptamolybdate and aniline in 10-30mL of deionized water, dropwise adding 1mol/L aqueous solution of hydrogen chloride under magnetic stirring, adjusting the pH value to 4-5, placing the mixed solution in an oil bath at 30-80 ℃ for reaction for more than 4-6 hours, filtering and cleaning the obtained precipitate to obtain a Mo precursor preliminarily, grinding the precursor, and carbonizing the precursor at 600 ℃ for 1-3 hours under a reducing atmosphere to obtain Mo2Sample C-600. Mo obtained in the example2Dispersing C-600 nanowires in an ethylene glycol solution, performing ultrasonic dispersion for 30-50 minutes in an ultrasonic cleaner at normal temperature to obtain a molybdenum carbide nanowire-ethylene glycol mixed solution, coating the mixed solution on a rinsed interdigital electrode by a silk screen printing technology, putting the platinum interdigital electrode coated with the cubic phase molybdenum carbide nanowire-ethylene glycol mixed solution into a vacuum oven, and drying under the conditions of vacuum and 60-100 ℃ for 8-12 hours toEthylene glycol is completely volatilized to form a stable molybdenum carbide film to cover the interdigital electrode sensing area, so that Mo is obtained2C-600 gas sensor.
Mo obtained in the example2The C-600 nanowire gas sensor is arranged in the detection device and is used for detecting SO at different temperatures and different concentrations2F2The gas-sensitive detection is carried out, the response curve of the sensor is shown in figure 5, and different SOs are detected under the normal temperature state2F2The concentration and the response value are all floated at about 1; SO at the same detection temperature except at normal temperature2F2The higher the gas concentration, the larger the response value; at the same concentration, the response tends to increase with the increase of the temperature. Wherein, at 50 ℃, the lowest successful detection of 150ppm SO can be realized2F2The response value was 1.13, and 30ppm SO was detected at 350 ℃ with minimum success2F2The response value was 1.1.
Example 6
Dissolving 1.24-4.15g of ammonium heptamolybdate and aniline in 10-30mL of deionized water, dropwise adding 1mol/L aqueous hydrogen chloride solution under magnetic stirring, adjusting the pH value to 4-5, placing the mixed solution in an oil bath at 30-80 ℃ for reaction for more than 4-6 hours, filtering and cleaning the obtained precipitate to obtain a Mo precursor preliminarily, grinding the precursor, and carbonizing the precursor at 700 ℃ for 1-3 hours under a reducing atmosphere to obtain Mo2Sample of C-700. Mo obtained in the example2Dispersing C-700 nanowires in an ethylene glycol solution, performing ultrasonic dispersion for 30-50 minutes in an ultrasonic cleaner at normal temperature to obtain a molybdenum carbide nanowire-ethylene glycol mixed solution, coating the mixed solution on a rinsed interdigital electrode by a silk screen printing technology, putting the platinum interdigital electrode coated with the cubic phase molybdenum carbide nanowire-ethylene glycol mixed solution into a vacuum oven, drying for 8-12 hours at the temperature of 60-100 ℃ in vacuum until ethylene glycol is completely volatilized, forming a stable molybdenum carbide film to cover an interdigital electrode sensing area, and obtaining Mo2C-700 gas sensor.
Mo obtained in the example2The C-700 nanowire gas sensor is arranged in the detection device and is used for detecting SO at different temperatures and different concentrations2F2The gas-sensitive detection is carried out, the response curve of the sensor is shown in figure 6, and different SO are respectively detected under the state of normal temperature to 100 DEG C2F2The concentration and the response value are all floated at about 1; at high temperatures (350 ℃), SO2F2The higher the gas concentration, the greater the degree of response. At 350 ℃, 150ppm of SO can be successfully detected at the lowest2F2The response value was 0.89.
The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (4)
1. A preparation method of a cubic phase molybdenum carbide nanowire gas sensor is characterized by comprising the following steps:
step one, preparing a cubic phase molybdenum carbide nanowire: dissolving a certain amount of ammonium heptamolybdate and aniline in deionized water, dropwise adding a certain molar mass of aqueous hydrogen chloride solution under magnetic stirring, placing the mixed solution in an oil bath at 30-80 ℃ for reaction for 4-6 hours, filtering and cleaning the precipitate to obtain a preliminary Mo precursor, grinding the precursor, and carbonizing at the temperature of 500-700 ℃ in a reducing atmosphere to obtain a cubic phase molybdenum carbide nanowire;
and secondly, ultrasonically washing a platinum interdigital electrode arranged in the gas sensor by using deionized water, dispersing the cubic-phase molybdenum carbide nanowire obtained in the first step in an ethylene glycol solution, ultrasonically dispersing for 30-50 minutes in an ultrasonic cleaner at normal temperature to obtain a molybdenum carbide nanowire-ethylene glycol mixed solution, coating the mixed solution on the cleanly washed interdigital electrode by using a screen printing technology, putting the platinum interdigital electrode coated with the cubic-phase molybdenum carbide nanowire-ethylene glycol mixed solution into a vacuum oven, drying for 8-12 hours at the temperature of 60-100 ℃ in vacuum until the ethylene glycol is completely volatilized, forming a stable molybdenum carbide film to cover an interdigital electrode sensing area, and obtaining the cubic-phase molybdenum carbide nanowire gas sensor.
2. The method for preparing the cubic phase molybdenum carbide nanowire gas sensor as claimed in claim 1, wherein the method comprises the following steps: in the first step, 1.24-4.15g of ammonium heptamolybdate and aniline are dissolved in 10-30mL of deionized water, 1mol/L of aqueous hydrogen chloride solution is dropwise added under magnetic stirring, and the pH value is adjusted to 4-5 to obtain a mixed solution.
3. The method for preparing the cubic phase molybdenum carbide nanowire gas sensor as claimed in claim 1, wherein the method comprises the following steps: and in the first step, the mixed solution is placed in an oil bath at the temperature of 30-80 ℃ for reaction for 4-6 hours, and the precipitate is filtered and cleaned to obtain a primary Mo precursor.
4. The use of the cubic phase molybdenum carbide nanowire gas sensor as claimed in any one of claims 1 to 3, wherein the cubic phase molybdenum carbide nanowire-based gas sensor is used for detecting SF6The method comprises the following specific steps of:
step 1, parameter setting: setting the working temperature of the cubic phase molybdenum carbide nanowire to be normal temperature (25 ℃) to 350 ℃, wherein the gas concentration is 10ppm to 300 ppm;
step 2, gas-sensitive testing: loading the cubic phase molybdenum carbide nanowire gas sensor into a testing device, and introducing inert gas helium into the testing device until the initial resistance value of molybdenum carbide is stable and is recorded as R0Then the gas to be measured is introduced immediately, and the resistance value after the resistance is stabilized is recorded as R1Calculating the relative variation S-R of the sensor resistance0/R1And the response capability of the cubic phase molybdenum carbide nanowire gas sensor to gas to be measured is reflected by the size of the sensor.
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