CN115015328A - N-pentanol gas sensor based on PtAu alloy nanocrystalline modified flower-shaped WO3 sensitive material and preparation method thereof - Google Patents
N-pentanol gas sensor based on PtAu alloy nanocrystalline modified flower-shaped WO3 sensitive material and preparation method thereof Download PDFInfo
- Publication number
- CN115015328A CN115015328A CN202210450061.2A CN202210450061A CN115015328A CN 115015328 A CN115015328 A CN 115015328A CN 202210450061 A CN202210450061 A CN 202210450061A CN 115015328 A CN115015328 A CN 115015328A
- Authority
- CN
- China
- Prior art keywords
- sensitive material
- ptau
- flower
- shaped
- ceramic tube
- 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.)
- Granted
Links
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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (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
Flower-shaped WO based on PtAu alloy nanocrystalline modification 3 An n-amyl alcohol gas sensor of sensitive material and a preparation method thereof belong to the technical field of semiconductor metal oxide gas sensors. In the present invention, PtAu alloy nanocrystals are synthesized using oleylamine, flower-like WO 3 Prepared by a simple hydrothermal method, and PtAu alloy nanocrystals are loaded to flower-shaped WO by a dipping method 3 Flower-shaped WO with PtAu alloy nanocrystalline modification prepared on surface 3 A sensitive material. The sensor is made of Al with a gold electrode on the outer surface 2 O 3 The ceramic pipe, the coated sensitive material and the Cr-Ni alloy heating wire. The n-amyl alcohol sensor has excellent gas-sensitive performance, and test results show that the response of the sensor to 20ppm n-amyl alcohol gas can reach 161.7, and the response speed is only 1 s. In addition, the sensor has good selectivity to n-amyl alcohol. The sensor is expected to realize the rapid detection of the n-amyl alcohol gas.
Description
Technical Field
The invention belongs to a semiconductorThe technical field of metal oxide gas sensors, in particular to flower-shaped WO based on PtAu alloy nanocrystalline modification 3 An n-amyl alcohol gas sensor of sensitive material and a preparation method thereof.
Background
Environmental pollution and health damage caused by the emission of Volatile Organic Compounds (VOCs) have attracted considerable attention over the past several decades. N-pentanol, a colorless, flammable liquid with off-flavors, is one of the most representative volatile organic compounds, which has a wide range of usage scenarios, including use in perfume production, medicine, and biofuels. When n-pentanol vapor is volatilized into the surrounding environment, it not only seriously pollutes the air but also poses a hazard to human health, for example, when the n-pentanol concentration exceeds 15.6ppm, it may irritate the skin and eyes of a human, damage the respiratory system and cause headache and nausea. In order to protect human health and monitor air pollution, it is important to accurately and timely detect n-pentanol in the environment. Common methods for detecting n-pentanol mainly include gas chromatography-mass spectrometry and fluorescence spectrometry. Although they have low detection limit and high accuracy, the detection instruments have large volume, high energy consumption and long detection period, thereby limiting the application of the detection instruments in air quality monitoring and environmental protection. In contrast, semiconductor Metal Oxide (MOS) based gas sensors have received extensive research and attention due to their advantages of low cost, small size, environmental protection, ease of manufacture, and real-time on-line monitoring.
Of all MOS materials, flower-like WO 3 Is a typical n-type semiconductor, and is an excellent candidate material for detecting n-pentanol due to its low cost, good stability, high electron mobility and good gas sensitivity. Because the carbon chain of the n-amyl alcohol is long and the relative molecular weight is large, the pure MOS-based n-amyl alcohol gas sensor generally has the problems of unsatisfactory response, slow recovery speed and the like. Multiple studies indicate that noble metal surface modification is an effective method for improving sensing performance. The noble metal Pt is widely applied to the field of gas sensitivity due to the excellent catalytic performance of the noble metal Pt, and researches show that the Pt can improve the response, accelerate the response speed and reduce the working temperature. Au as another commonly used noble metal elementElements have also been reported to enhance gas sensitivity to VOCs. Therefore, the bimetallic alloy nanocrystal formed of Pt and Au is expected to improve the response to amyl alcohol, improve the response speed and the recovery characteristics of the sensor.
Disclosure of Invention
The invention aims to provide flower-shaped WO modified based on PtAu alloy nanocrystals 3 An n-amyl alcohol gas sensor of sensitive material and a preparation method thereof.
Flower-shaped WO modified by PtAu alloy nanocrystals 3 As a sensitive material, the PtAu alloy nanocrystalline dissociates oxygen molecules and then overflows to WO 3 The surface can greatly increase the surface adsorbed oxygen content, which promotes the redox reaction that occurs on the surface of the sensitive material. In addition, since the work functions of Pt (5.65eV) and Au (5.1eV) are larger than those of WO 3 (4.56eV), therefore WO 3 The electrons in the PtAu alloy are lost to the PtAu alloy nano particles, and the process not only ensures that the WO is used 3 The expansion of the depletion layer also increases the electron density on the surface of the PtAu nano particle, thereby enhancing the capture capability to oxygen and being beneficial to improving the gas-sensitive response when detecting n-amyl alcohol gas. The sensor adopts a commercially available tubular structure sensor, has a simple manufacturing process and a small volume, and is beneficial to industrial mass production, so the sensor has important application value.
The flower-shaped WO based on PtAu alloy nanocrystalline modification 3 The n-amyl alcohol gas sensor of sensitive material is made of Al whose external surface is equipped with two parallel, ring-shaped and mutually-separated Au electrodes 2 O 3 Ceramic tube, sensitive material coated on Au electrode and ceramic tube outer surface, Al-positioned ceramic tube and method for manufacturing the same 2 O 3 The inside of the ceramic tube is provided with a Cr-Ni alloy heating wire for providing temperature for sensitive materials; the method is characterized in that: flower-shaped WO with sensitive material modified by PtAu alloy nanocrystalline 3 The sensitive material is prepared by the following steps:
(1) 1.035mL, 0.05g/mL of H 2 PtCl 6 ·6H 2 Aqueous O solution and 0.783mL of 0.05g/mL of AuCl 3 ·3H 2 Uniformly mixing the O water solution and uniformly performing ultrasonic treatment, and adding 9-10 mL of oleylamine and 1-2 mL of oleic acid into the mixture by using a liquid transfer gun at 50-6 mLStirring at 0 ℃ for 0.5-2.0 h, then heating to 140-150 ℃ at the speed of 1.5-3.0 ℃/min per minute, and reducing for 0.5-2.0 h under the protection of nitrogen; after cooling to room temperature, centrifugally washing the obtained product for 2-4 times by using a mixed solution of n-hexane and ethanol, and dispersing the obtained PtAu alloy nanocrystals into the n-hexane to obtain PtAu alloy nanocrystal colloid, wherein the concentration of the PtAu alloy nanocrystals is 6.61 mg/mL; the concentration calculation method of the PtAu alloy nanocrystalline comprises the following steps: dripping 0.3-0.5 mL of PtAu alloy nanocrystalline dispersed in n-hexane onto a clean glass sheet, drying, measuring the mass difference of the front and the back of the glass sheet to obtain the mass of the PtAu alloy nanocrystalline, and dividing the mass of the PtAu alloy nanocrystalline by the volume of a solution dripped on the glass sheet to obtain the concentration of the PtAu alloy nanocrystalline;
(2) 0.334g P123 (polyoxyethylene-polyoxypropylene-polyoxyethylene, purchased from Chinese pharmacopoeia) is dissolved in a mixed solution of 50-60 mL of anhydrous ethanol and 0.5-1 mL of water, vigorously stirred (800-1200 rpm) for 30-50 minutes, and 1.332g WCl is added to the mixed solution under continuous stirring 6 Until a clear yellow transparent solution is formed; then transferring the clear solution into a polytetrafluoroethylene reaction kettle, and keeping the temperature at 140-160 ℃ for 3-5 hours; after the reaction is finished and the temperature is cooled to room temperature, centrifuging and collecting the precipitate, and washing the precipitate for 4-6 times by using deionized water and ethanol alternately; finally, drying the precipitate at 50-70 ℃ overnight, and annealing in air at 350-450 ℃ for 1.5-3.0 hours to obtain flower-shaped WO 3 Powder;
(3) 100mg of flower-like WO 3 Adding the powder into 15-30 mL of n-hexane for ultrasonic dispersion for 20-40 minutes to obtain WO 3 A dispersion liquid; then adding 0.015-0.106 mL of PtAu alloy nanocrystalline colloid into WO 3 Performing ultrasonic treatment for 20-40 minutes in the dispersion liquid; finally, drying the PtAu alloy nano-crystal for 3 to 4 hours at the temperature of between 60 and 80 ℃ to evaporate n-hexane so as to obtain the PtAu alloy nano-crystal modified WO 3 Sensitive material (PtAu-WO) 3 )。
The invention relates to a flower-shaped WO modified based on PtAu alloy nanocrystals 3 The preparation method of the n-amyl alcohol sensor of the sensitive material comprises the following steps:
(1) flower-shaped WO modified by 50-100 mg of PtAu alloy nanocrystalline 3 Mixing the sensitive material with 0.05-0.1 mL of absolute ethyl alcohol, and performing ultrasonic treatment for 10-20 minutes to uniformly disperse the mixture to obtain slurry; then dipping the slurry by a brush to evenly coat the Al of which the outer surface is provided with two parallel annular Au electrodes which are separated from each other 2 O 3 The outer surface of the ceramic tube enables the sensitive material to completely cover the gold electrode, and the thickness of the sensitive material layer is 30-40 mu m;
(2) al obtained in the step (1) 2 O 3 Calcining the ceramic tube at 180-220 ℃ for 1.5-3.0 h to fix the sensitive material layer on the ceramic tube; then enabling the Cr-Ni alloy heating wire with the resistance value of 30-40 omega to penetrate through Al 2 O 3 Finally, the ceramic tube is welded on a hexagonal base according to an indirectly heated gas sensitive element inside the ceramic tube, so that flower-shaped WO based on PtAu alloy nanocrystalline modification is obtained 3 An n-amyl alcohol sensor of sensitive material.
Al 2 O 3 The ceramic tube has a length of 4.0 to 4.5mm, an outer diameter of 1.0 to 1.5mm and an inner diameter of 0.7 to 1.0 mm. The width of the Au electrodes is 0.3-0.6 mm, and the distance between the two Au electrodes is 2.0-2.5 mm.
Flower-shaped WO prepared by the invention based on PtAu alloy nanocrystalline modification 3 The n-amyl alcohol gas sensor of the sensitive material has the following advantages:
1. synthesizing PtAu alloy nanocrystalline by oleylamine coreduction method, and synthesizing WO by solvothermal method 3 A main material, finally loading PtAu alloy nano-crystals to WO by using an immersion method 3 The surface of the material is provided with sensitive materials, and the synthesis method is economical and simple;
2. the chemical sensitization of the PtAu alloy nanocrystalline greatly improves the WO 3 Adsorbed oxygen content of the surface, due to work function differences, WO 3 The loss of electrons further expands WO 3 The thickness of the depletion layer on the surface is increased, so that the response of the depletion layer to the n-amyl alcohol gas is greatly improved;
3. PtAu alloy nanocrystalline modified flower-shaped WO 3 The sensitive material shows high response and ultra-fast response speed to 20ppm n-amyl alcohol at 200 ℃;
4. the ceramic tube sensor structure sold in the market is adopted, the size is small, the process is simple, and mass production can be realized.
Drawings
FIG. 1: the flower-shaped WO based on PtAu alloy nanocrystalline modification 3 Sensitive material (PtAu-WO) 3 ) The structure of the n-amyl alcohol gas sensor is shown in the specification;
FIG. 2 is a schematic diagram: (a) TEM image of PtAu alloy nanocrystal, (b) XRD image of PtAu alloy nanocrystal;
FIG. 3: (a) pure WO 3 SEM picture of (a), (b) PtAu-WO 3 SEM picture of (1);
FIG. 4: flower-shaped WO 3 And flower-shaped WO modified by PtAu alloy nanocrystalline 3 (PtAu-WO 3 ) XRD pattern of (a);
FIG. 5: (a) pure WO 3 Dynamic response curve at 200 ℃ for 20ppm n-pentanol, (b) PtAu-WO 3 Dynamic response curve at 200 ℃ for 20ppm n-pentanol;
FIG. 6: pure WO 3 At 200 ℃ and PtAu-WO 3 A response curve to 1-20 ppm of n-pentanol at 200 ℃;
FIG. 7: pure WO 3 And PtAu-WO 3 Graph comparing selectivity at 200 ℃ for different interfering gases.
Shown in figure 1, flower-shaped WO modified based on PtAu alloy nanocrystals 3 The n-amyl alcohol gas sensor of the sensitive material structurally comprises a hexagonal base, a ceramic tube, the sensitive material, an Au electrode and a Cr-Ni heating wire; two gold electrodes and a Cr-Ni heating wire are welded on the hexagonal base through Pt wire leads, sensitive materials are coated on the outer surfaces of the ceramic tube and the gold electrodes, and the Cr-Ni heating wire penetrates through the interior of the ceramic tube.
As shown in fig. 2a, it can be seen that the nanocrystals are pseudo-spherical, with a size of about 5 nm; fig. 2b shows that the nanocrystals are in the platinum phase and the 2 θ of the PtAu alloy is shifted to a low angle compared to XRD of Pt, indicating that the lattice parameters are increased by the Au doped Pt lattice.
As shown in FIG. 3, the flower shape WO can be seen from FIG. 3a 3 Is micron-sized and is assembled by a plurality of nano sheets. FIG. 3b shows that the PtAu alloy nanocrystal pair WO is loaded 3 There is no influence on the quality of the product,the appearance is unchanged before and after loading.
As shown in FIG. 4, pure WO 3 And PtAu-modified WO 3 The XRD peak position and the peak intensity of the PtAu alloy are hardly changed, which shows that after the PtAu alloy nanocrystalline is introduced, the WO 3 No change in lattice parameter occurred.
As shown in FIG. 5, it can be seen from both comparative example (a) and example (b) that the resistance decreased when the sensor was exposed to n-pentanol gas, while WO modified with PtAu alloy 3 The reduction is more significant and the response speed is significantly improved, shortened to 1 s. When the sensor is placed in an air atmosphere, the resistance value can return to the initial state. Pure WO 3 And PtAu-modified WO 3 The working temperature is 200 ℃, and the working temperature is unchanged.
As shown in FIG. 6, the responsivity of the comparative example and the example to 1-20 ppm n-pentanol increases along with the increase of the concentration, and the PtAu modified WO 3 The responsivity of (A) is greater than that of pure WO at each concentration 3 The response to 20ppm n-amyl alcohol gas can reach 161.7, and the response has good linear relation.
FIG. 7 shows PtAu-modified WO 3 Good selectivity is shown for 20ppm of n-pentanol.
Note: the responsivity of the sensor is defined as the resistance value (R) in air between two gold electrodes a ) And resistance value (R) in n-pentanol g ) The ratio is S ═ R a /R g . During the test, a static test system is used for testing. And (3) placing the device in a 1L air chamber, injecting a certain amount of n-amyl alcohol gas inwards, observing and recording the resistance change of the n-amyl alcohol gas, and calculating to obtain a corresponding responsivity numerical value.
Detailed Description
Comparative example 1:
in the shape of flower WO 3 The n-amyl alcohol gas sensor is made of sensitive materials, and the specific manufacturing process is as follows:
1. 0.334g P123 (polyoxyethylene-polyoxypropylene-polyoxyethylene) was dissolved in a mixed solution of 54.8mL of anhydrous ethanol and 0.5mL of water, vigorously stirred for 40 minutes, and then 1.332g of WCl was added to the solution with continuous stirring 6 Until a clear yellow color is formedAnd (4) a transparent solution.
2. The clear solution was transferred to a teflon reaction kettle, which was held at 150 ℃ for 4 hours. After the reaction is finished and the temperature is cooled to room temperature, the precipitate is collected by centrifugation and is washed for 5 times by deionized water and absolute ethyl alcohol alternately. Finally, the precipitate was dried in an oven at 60 ℃ overnight and then annealed in air at 400 ℃ for 2 hours to give flower-like WO 3 Sensitive material powder.
3. 50mg of flower-like WO 3 The sensitive material powder is mixed with 0.1mL of absolute ethyl alcohol and is ultrasonically and uniformly mixed, and then a brush is used for dipping slurry to be uniformly coated on Al with two parallel, annular and mutually separated gold electrodes 2 O 3 The surface of the ceramic tube is covered by the sensitive material, and the thickness of the sensitive material is 35 mu m.
4. Mixing Al 2 O 3 Calcining the ceramic tube at 200 ℃ for 2h to fix the sensing layer on the ceramic tube; then, a Cr-Ni alloy heating wire with the resistance value of 35 omega is penetrated through Al 2 O 3 The ceramic tube is welded on a hexagonal base according to an indirectly heated gas sensitive element, thereby obtaining the flower-shaped WO 3 N-amyl alcohol sensor of sensitive material.
5. The sensitivity of the sensor to n-pentanol was tested at 200 ℃.
Example 1:
flower-shaped WO modified based on PtAu alloy nanocrystals 3 The n-amyl alcohol gas sensor of the sensitive material has the following specific manufacturing process:
1. 1.035mL, 0.05g/mL of H 2 PtCl 6 ·6H 2 Aqueous O solution and 0.783mL of 0.05g/mL of AuCl 3 ·3H 2 And uniformly mixing the O water solution and uniformly performing ultrasonic treatment. Then, the homogeneously mixed solution was transferred to a three-necked flask, 9.5mL oleylamine and 1.5mL oleic acid were added by using a pipette gun and then stirred at 60 ℃ for 1 hour, then heated to 150 ℃ at 2 ℃/min, and finally reduced under a nitrogen atmosphere for 1 hour. After cooling, collecting the obtained product, centrifugally washing the product for 3 times by using a mixed solution of normal hexane and absolute ethyl alcohol, and dispersing the obtained PtAu alloy nano-crystal into the normal hexane to obtain the PtAu alloy nano-crystalRice-grain colloid. The concentration calculation method of the PtAu alloy nanocrystalline comprises the following steps: and dripping 0.3mL of the PtAu alloy nanocrystalline dispersed in n-hexane onto a clean glass sheet, drying, measuring the mass difference of the front and the back of the glass sheet to obtain the mass of the PtAu alloy nanocrystalline, and dividing the mass of the PtAu alloy nanocrystalline by the volume of the solution dripped on the glass sheet to obtain the concentration of the PtAu alloy nanocrystalline of 6.61 mg/mL.
2. 0.334g P123 (polyoxyethylene-polyoxypropylene-polyoxyethylene) was dissolved in a mixed solution of 54.8mL of anhydrous ethanol and 0.5mL of water, vigorously stirred for 40 minutes, and then 1.332g of WCl was added to the solution with continuous stirring 6 Until a clear yellow transparent solution is formed. The clear solution was then transferred to a teflon reaction kettle, which was held at 150 ℃ for 4 hours. After the reaction is finished and the temperature is cooled to room temperature, the precipitate is collected by centrifugation and washed by deionized water and absolute ethyl alcohol alternately for 5 times. Finally, the precipitate was dried in an oven at 60 ℃ overnight and then annealed in air at 400 ℃ for 2 hours to give flower-like WO 3 Sensitive material powder.
3. 100mg of flower-like WO 3 Adding sensitive material powder into 20mL n-hexane, performing ultrasonic treatment for 30 minutes, and adding 0.0756mL PtAu alloy nanocrystalline colloid into dispersed flower-shaped WO 3 And (5) performing ultrasonic treatment for 30 minutes. Finally, the cells were collected by centrifugation and dried at 60 ℃ for 8 hours to obtain PtAu-modified WO 3 And (4) sensitive material.
4. WO modified with 50mg of PtAu alloy nanocrystals 3 Mixing the sensitive material of the micro-flowers with 0.1mL of absolute ethyl alcohol, performing ultrasonic treatment for 10 minutes to uniformly disperse the sensitive material of the micro-flowers to obtain slurry, dipping the slurry by a brush to uniformly coat the slurry on Al with two parallel gold electrodes which are separated from each other 2 O 3 The sensitive material completely covers the gold electrode on the surface of the ceramic tube; the thickness of the sensitive material is 35 μm.
5. Mixing Al 2 O 3 Calcining the ceramic tube at 200 ℃ for 2h to fix the sensing layer on the ceramic tube; then, a Cr-Ni alloy heating wire with the resistance value of 35 omega is penetrated through Al 2 O 3 The ceramic tube is welded to a hexagonal base according to the heater gas sensorThus obtaining flower-shaped WO modified based on PtAu alloy nanocrystals 3 An n-amyl alcohol sensor of sensitive material.
6. Testing PtAu alloy nanocrystalline modified flower-shaped WO at 200 DEG C 3 The sensor of the sensitive material has gas-sensitive response to the amyl alcohol.
Claims (3)
1. Flower-shaped WO based on PtAu alloy nanocrystalline modification 3 The n-amyl alcohol sensor of sensitive material is made of Al whose external surface is equipped with two parallel, ring-shaped and mutually-separated Au electrodes 2 O 3 Ceramic tube, sensitive material coated on Au electrode and ceramic tube outer surface, Al-positioned ceramic tube and method for manufacturing the same 2 O 3 The inside of the ceramic tube is provided with a Cr-Ni alloy heating wire for providing temperature for sensitive materials; the method is characterized in that: WO with PtAu alloy nanocrystalline modified as sensitive material 3 A sensitive material of micro-flowers of rice, and it is prepared by the following steps,
(1) 1.035mL, 0.05g/mL of H 2 PtCl 6 ·6H 2 Aqueous O solution and 0.783mL, 0.05g/mL of AuCl 3 ·3H 2 Uniformly mixing the O water solution, ultrasonically uniformly mixing, adding 9-10 mL of oleylamine and 1-2 mL of oleic acid by using a liquid transfer gun, stirring for 0.5-2.0 h at 50-60 ℃, then heating to 140-150 ℃ at the speed of 1.5-3.0 ℃/min per minute, and reducing for 0.5-2.0 h under the protection of nitrogen; after cooling to room temperature, centrifugally washing the obtained product for 2-4 times by using a mixed solution of n-hexane and ethanol, and dispersing the obtained PtAu alloy nanocrystals into the n-hexane to obtain PtAu alloy nanocrystal colloid, wherein the concentration of the PtAu alloy nanocrystals is 6.61 mg/mL;
(2) dissolving 0.334g polyoxyethylene-polyoxypropylene-polyoxyethylene in a mixed solution of 50-60 mL absolute ethanol and 0.5-1 mL water, vigorously stirring for 30-50 minutes, and adding 1.332g WCl to the mixed solution under continuous stirring 6 Until a clear yellow transparent solution is formed; then transferring the clear solution into a polytetrafluoroethylene reaction kettle, and keeping the temperature at 140-160 ℃ for 3-5 hours; after the reaction is finished and the temperature is cooled to room temperature, centrifuging and collecting precipitates, and washing the precipitates for 4-6 times by using deionized water and ethanol alternately; finally, drying the precipitate at 50-70 ℃ overnight, and then drying the precipitate at 350-45 DEG CAnnealing in air at 0 ℃ for 1.5-3.0 hours to obtain flower-shaped WO 3 Powder;
(3) 100mg of flower-like WO 3 Adding the powder into 15-30 mL of n-hexane for ultrasonic dispersion for 20-40 minutes to obtain WO 3 A dispersion liquid; then adding 0.015-0.106 mL of PtAu alloy nanocrystalline colloid into WO 3 Performing ultrasonic treatment for 20-40 minutes in the dispersion liquid; finally, drying at 60-80 ℃ for 3-4 hours to evaporate n-hexane, thereby obtaining PtAu alloy nanocrystalline modified WO 3 And (4) sensitive material.
2. Flower-shaped WO based on PtAu alloy nanocrystalline modification as claimed in claim 1 3 The n-amyl alcohol sensor of the sensitive material is characterized in that: al (Al) 2 O 3 The ceramic tube has a length of 4.0 to 4.5mm, an outer diameter of 1.0 to 1.5mm and an inner diameter of 0.7 to 1.0 mm.
The width of the Au electrodes is 0.3-0.6 mm, and the distance between the two Au electrodes is 2.0-2.5 mm.
3. Flower-like WO based on PtAu alloy nanocrystal modification as defined in claim 1 or 2 3 The preparation method of the n-amyl alcohol sensor of the sensitive material comprises the following steps:
(1) flower-shaped WO modified by 50-100 mg of PtAu alloy nanocrystalline 3 Mixing the sensitive material with 0.05-0.1 mL of absolute ethyl alcohol, and performing ultrasonic treatment for 10-20 minutes to uniformly disperse the mixture to obtain slurry; then dipping the slurry by a brush to evenly coat the Al with two parallel, annular and discrete Au electrodes on the outer surface 2 O 3 The outer surface of the ceramic tube is used for enabling the sensitive material to completely cover the gold electrode, and the thickness of the sensitive material layer is 30-40 mu m;
(2) al obtained in the step (1) 2 O 3 Calcining the ceramic tube at 180-220 ℃ for 1.5-3.0 h to fix the sensitive material layer on the ceramic tube; then enabling the Cr-Ni alloy heating wire with the resistance value of 30-40 omega to penetrate through Al 2 O 3 Finally, the ceramic tube is welded on a hexagonal base according to an indirectly heated gas sensitive element inside the ceramic tube, so that flower-shaped WO based on PtAu alloy nanocrystalline modification is obtained 3 N-pentanol sensing of sensitive materialsProvided is a device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210450061.2A CN115015328B (en) | 2022-04-26 | 2022-04-26 | N-amyl alcohol gas sensor based on PtAu alloy nanocrystalline modified flower-shaped WO3 sensitive material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210450061.2A CN115015328B (en) | 2022-04-26 | 2022-04-26 | N-amyl alcohol gas sensor based on PtAu alloy nanocrystalline modified flower-shaped WO3 sensitive material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115015328A true CN115015328A (en) | 2022-09-06 |
| CN115015328B CN115015328B (en) | 2023-07-04 |
Family
ID=83067926
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210450061.2A Active CN115015328B (en) | 2022-04-26 | 2022-04-26 | N-amyl alcohol gas sensor based on PtAu alloy nanocrystalline modified flower-shaped WO3 sensitive material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115015328B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116969510A (en) * | 2023-07-28 | 2023-10-31 | 深圳市深晨科技有限公司 | Preparation method of gas-sensitive material sensitive to trimethylamine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105891272A (en) * | 2016-04-12 | 2016-08-24 | 吉林大学 | N-butanol gas sensor based on mesoporous WO3 material supporting precious metal Au and preparation method of n-butanol gas sensor |
| CN108956715A (en) * | 2018-07-19 | 2018-12-07 | 东北大学 | A kind of Au@WO3Core-shell nanospheres and its preparation method and application |
| CN110993967A (en) * | 2020-01-08 | 2020-04-10 | 济南大学 | CeO supported by Pt-Ni binary alloy2Nanoparticles and method for preparing same |
-
2022
- 2022-04-26 CN CN202210450061.2A patent/CN115015328B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105891272A (en) * | 2016-04-12 | 2016-08-24 | 吉林大学 | N-butanol gas sensor based on mesoporous WO3 material supporting precious metal Au and preparation method of n-butanol gas sensor |
| CN108956715A (en) * | 2018-07-19 | 2018-12-07 | 东北大学 | A kind of Au@WO3Core-shell nanospheres and its preparation method and application |
| CN110993967A (en) * | 2020-01-08 | 2020-04-10 | 济南大学 | CeO supported by Pt-Ni binary alloy2Nanoparticles and method for preparing same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116969510A (en) * | 2023-07-28 | 2023-10-31 | 深圳市深晨科技有限公司 | Preparation method of gas-sensitive material sensitive to trimethylamine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115015328B (en) | 2023-07-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108732207B (en) | Sensitive material for formaldehyde detection and preparation method and application thereof | |
| Meng et al. | Sub-ppb detection of acetone using Au-modified flower-like hierarchical ZnO structures | |
| Huang et al. | Enhanced acetone-sensing properties to ppb detection level using Au/Pd-doped ZnO nanorod | |
| WO2018082585A1 (en) | Synthesis method for composite gas sensitive material of porous zinc oxide nanosheet loaded with a high-dispersion nano precious metal | |
| CN108663417B (en) | One kind being directed to low concentration of NO2The novel I n of gas2O3/Sb2O3Composite hollow nanotube gas sensitive | |
| CN109052453B (en) | ZnCo2O4/ZnO heterostructure composite gas sensitive material and preparation method thereof | |
| CN108872325A (en) | One kind being based on SnSe2/SnO2Nitrogen dioxide gas sensor, preparation process and the application of hetero-junctions | |
| Liu et al. | Highly sensitive and selective trimethylamine sensors based on WO3 nanorods decorated with Au nanoparticles | |
| CN111830089A (en) | Based on two shell shape Cu2N-propanol gas sensor of O-grade structure micron sphere sensitive material and preparation method thereof | |
| CN104950017A (en) | Gas sensor based on core-shell flower-ball-shaped ZnFe2O4 nanometer materials, preparing method and application thereof | |
| CN104502413B (en) | Copper oxide doped stannic oxide based hydrogen sulfide gas sensitive material as well as preparation and application | |
| CN115015328A (en) | N-pentanol gas sensor based on PtAu alloy nanocrystalline modified flower-shaped WO3 sensitive material and preparation method thereof | |
| CN111693579A (en) | Hydrogen sulfide gas detection method and sensor based on nanosheet composite membrane | |
| CN113740391A (en) | MOF-derived NiO-Co3O4Preparation method of acetone gas sensor | |
| CN113447535A (en) | Gas sensitive material, preparation method and application thereof, and gas sensor element | |
| Sun et al. | Low-temperature H 2 S gas sensor based on spherical Ag 3 PO 4-doped SnO 2 | |
| CN106186059B (en) | A kind of high sensitivity flower-like structure TiO2The preparation method of sensing material | |
| CN109592713B (en) | Tungsten trioxide hollow nanosphere semiconductor material and preparation method thereof, gas sensor and preparation method and application thereof | |
| CN110711863A (en) | AuPd alloy nanoparticle loaded 3DOM WO3Preparation method of (1) | |
| CN110879245A (en) | Preparation method of heavy metal ion nano sensitive material | |
| LU502328B1 (en) | Preparation method of ethanol gas sensor based on nanofiber material of core-shell structure | |
| CN113213528A (en) | SnO/SnO synthesized by adopting hydrothermal method2Method for preparing nano composite gas-sensitive material | |
| CN114920280A (en) | MOF-5-based derived ZnO nano-chain material and application thereof | |
| CN111929350A (en) | Hydrogen sulfide gas detection method and sensor based on hollow microsphere composite membrane | |
| Tian et al. | Influence of ammonia sources on the gas sensing properties of the direct grown ZnO nanomaterials |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |