CN113848238A - Composite material based on cerium oxide/graphene, preparation method and application thereof, and sulfuryl fluoride gas-sensitive sensor - Google Patents
Composite material based on cerium oxide/graphene, preparation method and application thereof, and sulfuryl fluoride gas-sensitive sensor Download PDFInfo
- Publication number
- CN113848238A CN113848238A CN202111119187.3A CN202111119187A CN113848238A CN 113848238 A CN113848238 A CN 113848238A CN 202111119187 A CN202111119187 A CN 202111119187A CN 113848238 A CN113848238 A CN 113848238A
- Authority
- CN
- China
- Prior art keywords
- graphene
- composite material
- cerium oxide
- cerium
- ethanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 82
- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 51
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000005935 Sulfuryl fluoride Substances 0.000 title claims abstract description 8
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 title claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 239000002244 precipitate Substances 0.000 claims abstract description 22
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 17
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 68
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims description 14
- 238000012360 testing method Methods 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 10
- 230000004044 response Effects 0.000 abstract description 10
- 230000035945 sensitivity Effects 0.000 abstract description 10
- 238000011084 recovery Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 45
- 239000000243 solution Substances 0.000 description 21
- 238000003756 stirring Methods 0.000 description 12
- 238000005303 weighing Methods 0.000 description 12
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 9
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 9
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 9
- 239000002245 particle Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- YNAAFGQNGMFIHH-UHFFFAOYSA-N ctk8g8788 Chemical class [S]F YNAAFGQNGMFIHH-UHFFFAOYSA-N 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a cerium oxide/graphene-based composite material, a preparation method and application thereof, and a sulfuryl fluoride gas sensor, and relates to the field of gas detection. The preparation method comprises the following steps: s1, dispersing a cerium source, sodium hydroxide and sodium dodecyl sulfate in a solvent to prepare an initial solution; s2, dissolving graphene in deionized water, and performing ultrasonic treatment to form a graphene suspension; s3, uniformly mixing the graphene suspension with the initial solution, and calcining to obtain a solid-liquid mixture; and S4, collecting the precipitate in the solid-liquid mixture, cleaning and drying the precipitate, and performing secondary calcination to obtain the cerium oxide/graphene composite material. Cerium oxide/graphene composite material prepared by the method is used for SO2F2The gas has high sensitivity, and has higher sensitivity and stable cycle performance when being used as a sensitive layer in a gas sensor, and the response rate and the recovery rate are improved.
Description
Technical Field
The invention relates to the field of gas detection, in particular to a cerium oxide/graphene-based composite material, a preparation method and application thereof, and a sulfuryl fluoride gas sensor.
Background
Gas Insulated Switchgear (GIS) is often used in power systems, but GIS has a partial discharge phenomenon, which is a sign of performance degradation of gas insulated electrical equipment. When partial discharge occurs, internal SF6The gas is decomposed to generate a plurality of fluorine sulfides which further react with moisture and oxygen mixed in the GIS to generate SO2F2Gas, the partial discharge condition of GIS, especially SO, can be judged by detecting the characteristic component gas2F2The qualitative and quantitative detection of the GIS plays a critical role in judging the GIS insulation performance. SO SO2F2The research on the gas-sensitive performance has great practical significance for the safe construction and use of the power system.
Disclosure of Invention
The invention provides a cerium oxide/graphene-based composite material, a preparation method and application thereof, and a gas sensor, SO as to improve SO (sulfur oxide) of the gas sensor2F2Sensitivity of gas detection.
In order to solve the above technical problems, an object of an embodiment of the present invention is to provide a method for preparing a cerium oxide/graphene-based composite material, including the following steps:
s1, dispersing a cerium source, sodium hydroxide and sodium dodecyl sulfate in a solvent to prepare an initial solution;
s2, dissolving graphene in deionized water, and performing ultrasonic treatment to form a graphene suspension;
s3, uniformly mixing the graphene suspension with the initial solution, and calcining to obtain a solid-liquid mixture;
and S4, collecting the precipitate in the solid-liquid mixture, cleaning and drying the precipitate, and performing secondary calcination to obtain the cerium oxide/graphene composite material.
By adopting the scheme, the cerium source is dispersed and dissolved by using sodium hydroxide, and the lauryl sodium sulfate is fully dissolved, SO that cerium source particles are uniformly dispersed in the solution and the particle surfaces are not bonded, the graphene is uniformly dispersed and the particle surfaces are not bonded by ultrasonically treating the aqueous solution containing the graphene, the graphene particles and the cerium source are combined to form PN junctions in the heat treatment process, the surface performance of the precipitated particles is repaired after calcination, and the finally prepared cerium oxide/graphene composite material is used for treating SO2F2Has sensitivity and can be applied to the gas sensor for detecting SO2F2Gas, sensitivity is higher.
Preferably, in the S3, the calcining temperature is 150-180 ℃, and the calcining time is 10-14 h; in the S4, the calcining temperature is 300-400 ℃, and the calcining time is 2-4 h.
Preferably, in S1, the cerium source is cerium nitrate hexahydrate, and the solvent is an ethanol solution.
Preferably, in the S1, the solvent is prepared from ethanol and deionized water in a volume ratio of 1: 1, the ethanol is added by adding 10mL of ethanol into every 1mmoL of cerium source, and the molar ratio of the cerium source to the sodium hydroxide is 1: 5, the sodium dodecyl sulfate accounts for 0.0125 w/v% of the ethanol.
Preferably, in S2, the mass ratio of the graphene to the cerium source is 1: (200-300).
By adopting the scheme, the mass ratio of the graphene to the cerium source is limited to 1: the ratio of (200) -300) can ensure that the cerium oxide/graphene composite material with PN junction is finally generated, and the material pair SO2F2The sensitivity performance of the sensor is better.
Preferably, in S4, the washing is to mix the precipitate in the solid-liquid mixture with ethanol and deionized water, respectively, and remove the supernatant by centrifugation.
Preferably, in the step S4, the drying is to dry the washed precipitate at a temperature of 60 ℃ to 80 ℃ for 48h to 60 h.
In order to solve the above technical problems, a second object of the embodiments of the present invention is to provide a cerium oxide/graphene-based composite material, which is prepared by the above preparation method of the cerium oxide/graphene-based composite material.
In order to solve the technical problem, a third object of the embodiments of the present invention is to provide an application of a cerium oxide/graphene-based composite material, in which the cerium oxide/graphene-based composite material is dissolved in ethanol and then coated on the surface of an interdigital electrode of a gas sensor to form a sensitive layer.
In order to solve the technical problem, an object of the fourth embodiment of the present invention is to provide a sulfuryl fluoride gas sensor, which includes an interdigital electrode, wherein a sensitive layer is attached to a surface of the interdigital electrode, the sensitive layer is a cerium oxide/graphene composite material, and the cerium oxide/graphene composite material is prepared by the above preparation method of the cerium oxide/graphene-based composite material.
By adopting the scheme, the cerium oxide/graphene is used as the sensitive layer of the gas sensor to SO2F2The gas has higher sensitivity, higher response rate and recovery rate, and stable and good cycle performance.
Preferably, the optimal test temperature of the gas sensor is 50 ℃, and the optimal test relative humidity is 40%.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
1. the cerium source and the graphene are combined to form a PN junction in the heat treatment process, SO that the finally prepared cerium oxide/graphene composite material is used for treating SO2F2Has higher sensitivity, and can be applied to the gas sensor for detecting SO2F2Gas, using the cerium oxide/graphene as a sensitive layer of the gas sensor, and reacting with SO2F2The gas sensitivity is high, the response rate and the recovery rate are high, and the gas has stable and good cycle performance and high sensitivity.
Drawings
FIG. 1: the EDX detection result of the composite material based on cerium oxide graphene in embodiment 1 of the present invention;
FIG. 2: the invention is compared with an SO gas sensor pair in an application example2F2The response result of the gas;
FIG. 3: in the application example of the invention, the sulfuryl fluoride gas sensor is used for detecting SO2F2The response result of the gas;
FIG. 4: the schematic diagram of the PN junction generated by the composite material based on the cerium oxide graphene in the embodiment of the invention is shown.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A composite material based on cerium oxide graphene comprises the following preparation steps:
s1, respectively weighing 40mL of ethanol and 40mL of deionized water, mixing, and uniformly stirring to obtain an ethanol solution;
s2, weighing Ce (NO)3)3.6H2Dissolving 0 (cerous nitrate hexahydrate) in an ethanol solution, then adding sodium hydroxide, and stirring until the cerous nitrate is fully dissolved;
wherein 10mL of ethanol is added into 1mmoL of cerous nitrate hexahydrate, and the molar ratio of the cerous nitrate hexahydrate to the sodium hydroxide is 1: 5, the adding amount of the cerous nitrate hexahydrate is 1.74g, and the adding amount of the sodium hydroxide is 0.8 g;
s3, weighing sodium dodecyl sulfate, adding the sodium dodecyl sulfate into the solution obtained in the step S2, and stirring until the sodium dodecyl sulfate is fully dissolved to obtain an initial solution;
wherein 1g of sodium dodecyl sulfate is added into each 40mL of ethanol, and the specific addition amount of the sodium dodecyl sulfate is 1 g;
s4, weighing graphene, dissolving the graphene in 1ml of deionized water, and performing ultrasonic treatment for 6 hours to obtain a graphene suspension;
wherein the mass ratio of the graphene to the cerium nitrate is 1: 253, the specific addition amount of graphene is 0.00689 g;
s5, adding the graphene suspension into the initial solution, stirring and mixing uniformly, adding into a polytetrafluoroethylene lining reaction kettle, and reacting for 12 hours at the temperature of 160 ℃ to obtain a solid-liquid mixture;
s6, filtering and collecting precipitates in the solid-liquid mixture, alternately cleaning the precipitates for 10 times by using ethanol and deionized water, centrifuging to remove supernatant, controlling the centrifugation speed to be 5000r/min and the centrifugation time to be 5min to remove organic or inorganic impurities, and drying the cleaned precipitates in a drying box at 60 ℃ for 48 h;
and S7, grinding the dried precipitate, and calcining for 2 hours at the temperature of 300 ℃ to obtain the cerium oxide/graphene composite material.
Example two
A composite material based on cerium oxide graphene comprises the following preparation steps:
s1, respectively weighing 60mL of ethanol and 60mL of deionized water, mixing, and uniformly stirring to obtain an ethanol solution;
s2, weighing Ce (NO)3)3.6H2Dissolving 0 (cerous nitrate hexahydrate) in an ethanol solution, then adding sodium hydroxide, and stirring until the cerous nitrate is fully dissolved;
wherein 10mL of ethanol is added into 1mmoL of cerous nitrate hexahydrate, and the molar ratio of the cerous nitrate hexahydrate to the sodium hydroxide is 1: 5, the adding amount of the cerous nitrate hexahydrate is specifically 2.65g, and the adding amount of the sodium hydroxide is specifically 1.22 g;
s3, weighing sodium dodecyl sulfate, adding the sodium dodecyl sulfate into the solution obtained in the step S2, and stirring until the sodium dodecyl sulfate is fully dissolved to obtain an initial solution;
wherein 1g of sodium dodecyl sulfate is added into each 40mL of ethanol, and the specific addition amount of the sodium dodecyl sulfate is 1.5 g;
s4, weighing graphene, dissolving the graphene in 1ml of deionized water, and performing ultrasonic treatment for 6 hours to obtain a graphene suspension;
wherein the mass ratio of the graphene to the cerium nitrate is 1: 200, wherein the specific addition amount of the graphene is 0.01325 g;
s5, adding the graphene suspension into the initial solution, stirring and mixing uniformly, adding into a polytetrafluoroethylene lining reaction kettle, and reacting for 14 hours at the temperature of 150 ℃ to obtain a solid-liquid mixture;
s6, filtering and collecting precipitates in the solid-liquid mixture, alternately cleaning the precipitates for 10 times by using ethanol and deionized water, centrifuging to remove supernatant, controlling the centrifugation speed to be 5000r/min and the centrifugation time to be 5min to remove organic or inorganic impurities, and drying the cleaned precipitates for 54h in a drying box at 70 ℃;
and S7, grinding the dried precipitate, and calcining for 3 hours at the temperature of 400 ℃ to obtain the cerium oxide/graphene composite material.
EXAMPLE III
A composite material based on cerium oxide graphene comprises the following preparation steps:
s1, respectively weighing 80mL of ethanol and 80mL of deionized water, mixing, and uniformly stirring to obtain an ethanol solution;
s2, weighing Ce (NO)3)3.6H2Dissolving 0 (cerous nitrate hexahydrate) in an ethanol solution, then adding sodium hydroxide, and stirring until the cerous nitrate is fully dissolved;
wherein 10mL of ethanol is added into 1mmoL of cerous nitrate hexahydrate, and the molar ratio of the cerous nitrate hexahydrate to the sodium hydroxide is 1: 5, the adding amount of the cerous nitrate hexahydrate is specifically 3.54g, and the adding amount of the sodium hydroxide is specifically 1.63 g;
s3, weighing sodium dodecyl sulfate, adding the sodium dodecyl sulfate into the solution obtained in the step S2, and stirring until the sodium dodecyl sulfate is fully dissolved to obtain an initial solution;
wherein 1g of sodium dodecyl sulfate is added into each 40mL of ethanol, and the specific addition amount of the sodium dodecyl sulfate is 2 g;
s4, weighing graphene, dissolving the graphene in 1ml of deionized water, and performing ultrasonic treatment for 6 hours to obtain a graphene suspension;
wherein the molar ratio of the graphene to the cerium nitrate is 1: 300, the specific addition amount of the graphene is 0.0118 g;
s5, adding the graphene suspension into the initial solution, stirring and mixing uniformly, adding into a polytetrafluoroethylene lining reaction kettle, and reacting for 10 hours at the temperature of 180 ℃ to obtain a solid-liquid mixture;
s6, filtering and collecting precipitates in the solid-liquid mixture, alternately cleaning the precipitates for 10 times by using ethanol and deionized water, centrifuging and removing supernate, controlling the centrifugation speed to be 5000r/min and the centrifugation time to be 5min so as to remove organic or inorganic impurities, and drying the cleaned precipitates in a drying box at 80 ℃ for 60 h;
and S7, grinding the dried precipitate, and calcining for 4 hours at the temperature of 300 ℃ to obtain the cerium oxide/graphene composite material.
Application examples 1 to 3
A sulfuryl fluoride gas sensor comprises an interdigital electrode and a sensitive layer attached to the surface of the interdigital electrode, wherein the sensitive layer is a cerium oxide/graphene composite material prepared in the embodiment 1-3, the cerium oxide/graphene composite material is mixed with ethanol, dissolved, ground into slurry and coated on the surface of the interdigital electrode to form the sensitive layer, and the sensitive layer can be used for detecting SO2F2Gas, the optimum test temperature is 50 ℃, and the optimum test relative humidity is 40%.
Comparative application example 1
A gas sensor comprises an interdigital electrode and a sensitive layer attached to the surface of the interdigital electrode, wherein the sensitive layer is cerium oxide, a cerium oxide material and ethanol are mixed, dissolved, ground into slurry and then coated on the surface of the interdigital electrode to form the sensitive layer.
Performance test
1. The cerium oxide/graphene composite material obtained in example 1 is subjected to EDX detection, and the detection result is shown in fig. 1, and the detection result shows that the cerium oxide/graphene composite material has carbon element, cerium element and oxygen element, and is uniformly distributed, which indicates that the cerium oxide/graphene composite material obtained in example 1 is successfully compounded.
2. Gas-sensitive test: respectively carrying out gas-sensitive test on the corresponding application example 1 and the comparative application example 1, wherein the gas-sensitive test adopts a CGS-MT test system and a dynamic gas distribution method and adopts SF6For background gas, the inductive response (Sr) to the target gas is defined as Ra/Rg, where Ra and Rg are respectively the sensor at SF6(background gas) and target gas (SO)2F2) Resistance in the presence of, SO2F2The flush amount of (2) was 100 ppm. In the CGS-MT operation, the gas-sensitive test temperature is 50 ℃, the relative humidity is 40 percent, the nitrogen is firstly introduced to clean the chamber, and then SF is introduced6Introducing gas to be detected after its resistance value is stable, repeating SF after its resistance value is stable6The cycle stability can be tested in comparison with the operation of the gas to be detected, and the detection result of the application example 1 is shown in fig. 2, and the detection result of the application example 1 is shown in fig. 3.
From the results shown in FIGS. 2-3, it can be seen that when a pure cerium oxide material is used as the sensitive layer, the gas sensor is sensitive to SO2F2The response value (Ra/Rg) of the sensor is 1.2, and the stability of the sensitive layer in the circulating process is poor; when the cerium oxide/graphene composite material obtained in embodiment 1 of the present application is used as a sensitive layer, the gas sensor is sensitive to SO2F2The response value (Ra/Rg) of the sensor is 2.5, the sensitivity is high, the sensitive layer has stable and good cycle performance, the response time is 300s, the recovery time is 50s, the response speed is high, and the hypothesis is that the performance of the gas sensor is improved because a PN junction shown in a figure 4 is formed between cerium oxide and graphene.
The above-mentioned embodiments are provided to further explain the objects, technical solutions and advantages of the present invention in detail, and it should be understood that the above-mentioned embodiments are only examples of the present invention and are not intended to limit the scope of the present invention. It should be understood that any modifications, equivalents, improvements and the like, which come within the spirit and principle of the invention, may occur to those skilled in the art and are intended to be included within the scope of the invention.
Claims (10)
1. A preparation method of a cerium oxide/graphene-based composite material is characterized by comprising the following steps:
s1, dispersing a cerium source, sodium hydroxide and sodium dodecyl sulfate in a solvent to prepare an initial solution;
s2, dissolving graphene in deionized water, and performing ultrasonic treatment to form a graphene suspension;
s3, uniformly mixing the graphene suspension with the initial solution, and calcining to obtain a solid-liquid mixture;
and S4, collecting the precipitate in the solid-liquid mixture, cleaning and drying the precipitate, and performing secondary calcination to obtain the cerium oxide/graphene composite material.
2. The method for preparing the cerium oxide/graphene-based composite material according to claim 1, wherein in the step S3, the calcination temperature is 150-180 ℃, and the calcination time is 10-14 h; in the S4, the calcining temperature is 300-400 ℃, and the calcining time is 2-4 h.
3. The method of claim 1, wherein in the step of S1, the cerium source is cerium nitrate hexahydrate, and the solvent is ethanol solution.
4. The method for preparing a cerium oxide/graphene-based composite material according to claim 1, wherein in the step S1, the solvent is prepared from ethanol and deionized water in a volume ratio of 1: 1, the ethanol is added by adding 10mL of ethanol into every 1mmoL of cerium source, and the molar ratio of the cerium source to the sodium hydroxide is 1: 5, the sodium dodecyl sulfate accounts for 0.0125 w/v% of the ethanol.
5. The method for preparing a cerium oxide/graphene-based composite material according to claim 1 or 4, wherein in the step S2, the mass ratio of the graphene to the cerium source is 1: (200-300).
6. The method of claim 1, wherein in step S4, the washing is to mix the precipitate in the solid-liquid mixture with ethanol and deionized water, respectively, and remove the supernatant by centrifugation; and the drying is to dry the washed precipitate for 48 to 60 hours at the temperature of between 60 and 80 ℃.
7. A cerium oxide/graphene-based composite material, which is prepared by the preparation method of the cerium oxide/graphene-based composite material according to any one of claims 1 to 6.
8. The application of the cerium oxide/graphene-based composite material is characterized in that the cerium oxide/graphene-based composite material according to claim 7 is dissolved in ethanol and then coated on the surface of an interdigital electrode of a gas sensor to form a sensitive layer.
9. A sulfuryl fluoride gas sensor comprises an interdigital electrode, and is characterized in that a sensitive layer is attached to the surface of the interdigital electrode, the sensitive layer is a cerium oxide/graphene composite material, and the cerium oxide/graphene composite material is prepared by the preparation method of the cerium oxide/graphene-based composite material according to any one of claims 1 to 6.
10. The gas sensor of claim 9, wherein the gas sensor has an optimal test temperature of 50 ℃ and an optimal test relative humidity of 40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111119187.3A CN113848238A (en) | 2021-09-24 | 2021-09-24 | Composite material based on cerium oxide/graphene, preparation method and application thereof, and sulfuryl fluoride gas-sensitive sensor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111119187.3A CN113848238A (en) | 2021-09-24 | 2021-09-24 | Composite material based on cerium oxide/graphene, preparation method and application thereof, and sulfuryl fluoride gas-sensitive sensor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113848238A true CN113848238A (en) | 2021-12-28 |
Family
ID=78979615
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111119187.3A Pending CN113848238A (en) | 2021-09-24 | 2021-09-24 | Composite material based on cerium oxide/graphene, preparation method and application thereof, and sulfuryl fluoride gas-sensitive sensor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113848238A (en) |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103611523A (en) * | 2013-11-08 | 2014-03-05 | 南京大学 | Preparation method of high-dispersion lamellar nanometer ceric oxide/graphene composite material |
| CN104458826A (en) * | 2014-10-28 | 2015-03-25 | 大连理工大学 | Novel ammonia sensor and preparation technology thereof |
| CN104807860A (en) * | 2014-12-23 | 2015-07-29 | 郑州轻工业学院 | Flower-like nano-WO3/graphene composite gas-sensitive material and preparation method and application thereof |
| CN105181755A (en) * | 2015-08-24 | 2015-12-23 | 大连理工大学 | Ammonia gas sensor and preparation technology thereof |
| CN105259218A (en) * | 2015-10-28 | 2016-01-20 | 上海交通大学 | Zinc oxide nanowire-graphene gas sensor and preparation method thereof |
| US20160218353A1 (en) * | 2013-09-09 | 2016-07-28 | Ajou University Industry-Academic Cooperation Foun Dation | Method for preparing metal oxide-graphene nanocomposite and method for preparing electrode using metal oxide-graphene nanocomposite |
| CN106483169A (en) * | 2016-09-18 | 2017-03-08 | 西安交通大学 | A kind of high sensitivity gas sensor nano Ce O2The preparation method of/graphene composite material |
| CN109060892A (en) * | 2018-06-26 | 2018-12-21 | 西安交通大学 | SF based on graphene composite material sensor array6Decompose object detecting method |
| CN110095574A (en) * | 2019-05-06 | 2019-08-06 | 山东科技大学 | Acetylacetone,2,4-pentanedione gas sensitive material and the preparation method and application thereof |
| CN110498405A (en) * | 2019-08-21 | 2019-11-26 | 南京倍格电子科技有限公司 | A kind of graphene/tin oxide composite air-sensitive material and preparation method thereof |
| CN112798661A (en) * | 2020-12-31 | 2021-05-14 | 广东电网有限责任公司电力科学研究院 | SO (SO)2F2Gas sensor |
| CN112961653A (en) * | 2021-02-07 | 2021-06-15 | 广西立之亿新材料有限公司 | Preparation method of nano cerium oxide-graphene composite particles |
| CN113155913A (en) * | 2021-04-21 | 2021-07-23 | 浙江大学 | Gas sensor for detecting sulfur hexafluoride decomposition product and preparation method thereof |
-
2021
- 2021-09-24 CN CN202111119187.3A patent/CN113848238A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160218353A1 (en) * | 2013-09-09 | 2016-07-28 | Ajou University Industry-Academic Cooperation Foun Dation | Method for preparing metal oxide-graphene nanocomposite and method for preparing electrode using metal oxide-graphene nanocomposite |
| CN103611523A (en) * | 2013-11-08 | 2014-03-05 | 南京大学 | Preparation method of high-dispersion lamellar nanometer ceric oxide/graphene composite material |
| CN104458826A (en) * | 2014-10-28 | 2015-03-25 | 大连理工大学 | Novel ammonia sensor and preparation technology thereof |
| CN104807860A (en) * | 2014-12-23 | 2015-07-29 | 郑州轻工业学院 | Flower-like nano-WO3/graphene composite gas-sensitive material and preparation method and application thereof |
| CN105181755A (en) * | 2015-08-24 | 2015-12-23 | 大连理工大学 | Ammonia gas sensor and preparation technology thereof |
| CN105259218A (en) * | 2015-10-28 | 2016-01-20 | 上海交通大学 | Zinc oxide nanowire-graphene gas sensor and preparation method thereof |
| CN106483169A (en) * | 2016-09-18 | 2017-03-08 | 西安交通大学 | A kind of high sensitivity gas sensor nano Ce O2The preparation method of/graphene composite material |
| CN109060892A (en) * | 2018-06-26 | 2018-12-21 | 西安交通大学 | SF based on graphene composite material sensor array6Decompose object detecting method |
| CN110095574A (en) * | 2019-05-06 | 2019-08-06 | 山东科技大学 | Acetylacetone,2,4-pentanedione gas sensitive material and the preparation method and application thereof |
| CN110498405A (en) * | 2019-08-21 | 2019-11-26 | 南京倍格电子科技有限公司 | A kind of graphene/tin oxide composite air-sensitive material and preparation method thereof |
| CN112798661A (en) * | 2020-12-31 | 2021-05-14 | 广东电网有限责任公司电力科学研究院 | SO (SO)2F2Gas sensor |
| CN112961653A (en) * | 2021-02-07 | 2021-06-15 | 广西立之亿新材料有限公司 | Preparation method of nano cerium oxide-graphene composite particles |
| CN113155913A (en) * | 2021-04-21 | 2021-07-23 | 浙江大学 | Gas sensor for detecting sulfur hexafluoride decomposition product and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111422840B (en) | Phosphorus/graphene three-dimensional aerogel material and preparation method and application thereof | |
| CN102631890A (en) | Preparation method of modified fly ash adsorbent | |
| CN111589473B (en) | Regeneration and resource utilization method of thallium-poisoned SCR denitration catalyst | |
| CN103887488A (en) | Preparation method of peach-kernel-shaped SnO2-graphene-carbon composite material for lithium ion battery | |
| CN103832996A (en) | Graphene/carbon nano-tube composite material, preparation method and application thereof | |
| CN104979105A (en) | Nitrogen-doped porous carbon material, preparation method and applications | |
| CN109860526A (en) | The preparation method of graphite type material doping metals oxalates lithium battery composite negative pole material | |
| CN108545777A (en) | A kind of molybdenum disulfide/indium oxide quaternary gas sensitive and preparation method thereof of antimony-cerium modification | |
| CN111774045A (en) | Regeneration method of diatomite adsorbent | |
| CN102390832B (en) | Method for treating waste silicon powder produced in trichlorosilane synthesis process | |
| CN113848238A (en) | Composite material based on cerium oxide/graphene, preparation method and application thereof, and sulfuryl fluoride gas-sensitive sensor | |
| JP7117325B2 (en) | Method for producing vanadate | |
| CN110034293B (en) | L iMn2O4Preparation method of ternary cathode material for coated lithium ion battery | |
| CN105233797A (en) | Method for preparing sewage adsorbent from waste battery carbon material | |
| CN114408906B (en) | Method for purifying coal-based graphite and simultaneously preparing fluorinated graphene | |
| CN104148023B (en) | High-efficiency adsorbent of a kind of heavy metal lead ion and preparation method thereof and application | |
| CN103832995A (en) | Graphene/carbon nano-tube composite material, preparation method and application thereof | |
| CN108554365A (en) | A kind of uranium absorption agent and preparation method thereof | |
| CN105195083A (en) | Method for modifying ground calcium carbonate with sodium chloride to prepare heavy metal adsorbent | |
| CN102580674B (en) | Method for preparing mercury removal agent by utilizing modified waste tire pyrolysis residue | |
| CN111974361B (en) | Magnetic polydopamine hexavalent chromium reduction trapping agent based on sludge carrier and preparation method thereof | |
| CN112837947B (en) | Nitrogen and sulfur co-doped layered porous carbon hybrid material prepared from inorganic-cellulose raw material, and preparation and application thereof | |
| CN112678822A (en) | Preparation method of super activated carbon | |
| CN110184450A (en) | A method of processing arsenic scum | |
| CN111943189A (en) | Method for purifying graphite from waste cathode carbon block |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |