CN114813854A - Acetone sensor, preparation method and detection method - Google Patents
Acetone sensor, preparation method and detection method Download PDFInfo
- Publication number
- CN114813854A CN114813854A CN202210309012.7A CN202210309012A CN114813854A CN 114813854 A CN114813854 A CN 114813854A CN 202210309012 A CN202210309012 A CN 202210309012A CN 114813854 A CN114813854 A CN 114813854A
- Authority
- CN
- China
- Prior art keywords
- acetone
- ceramic tube
- doped
- gas
- sensor
- 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
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
-
- 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
-
- 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
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)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
本发明属于气体传感器制备技术领域，公开了一种丙酮传感器、制备方法及检测方法，包括：(1)以硝酸铁为金属盐，异丙醇/甘油的混合溶液为溶剂，水杨酸钠为表面活性剂，通过一步化学水热法成功制备Pt掺杂的α‑Fe2O3介孔微球；(2)按照旁热式器件工艺涂覆材料、组装、焊接完成基于Pt掺杂的α‑Fe2O3传感器的制备。本发明通过Pt的掺杂，提高了α‑Fe2O3气体传感器的灵敏度，测试结果表明利用本发明方法制备的基于Pt掺杂的α‑Fe2O3介孔微球材料的传感器对100ppm丙酮气体在最佳工作温度(175℃)下的灵敏度为105，可实现对丙酮的有效检测。本发明合成方法简单，成本低廉。
The invention belongs to the technical field of gas sensor preparation, and discloses an acetone sensor, a preparation method and a detection method, comprising: (1) using ferric nitrate as a metal salt, a mixed solution of isopropanol/glycerol as a solvent, and sodium salicylate as a Surfactant, Pt-doped α-Fe 2 O 3 mesoporous microspheres were successfully prepared by one-step chemical hydrothermal method; (2) Pt-doped α-based α-Fe 2 O 3 was completed by coating materials, assembling and welding according to the side-heating device process. ‑ Preparation of Fe 2 O 3 sensors. The present invention improves the sensitivity of the α-Fe 2 O 3 gas sensor through the doping of Pt, and the test results show that the sensor based on the Pt-doped α-Fe 2 O 3 mesoporous microsphere material prepared by the method of the present invention is suitable for 100ppm The sensitivity of acetone gas at the optimum working temperature (175℃) is 105, which can realize the effective detection of acetone. The synthesis method of the invention is simple and the cost is low.
Description
Technical Field
The invention belongs to the technical field of gas sensor preparation, and particularly relates to an acetone sensor, a preparation method and a detection method.
Background
At present, acetone is widely applied to organic solvents and chemical plant raw materials, and is a toxic and harmful organic solvent. Acetone can irritate nose and throat, and once the concentration exceeds 450mg/m 3 (173ppm), headache, dizziness and nervous system injury can be caused. Meanwhile, the detection of acetone in the breath is a noninvasive, rapid and effective diabetes diagnosis method. In order to prevent acetone leakage and effectively detect diabetes, it is important and urgent to detect acetone quickly and accurately.
Semiconductor Metal Oxide (MOS) based gas sensors have excellent sensing performance and are widely used for the detection of Volatile Organic Compounds (VOCs), such as methanol, ethanol, ammonia, acetone, and hydrogen sulfide. Compared with other gas detection methods, the method has the advantages of low cost, simple manufacture, easy integration and the like. alpha-Fe 2 O 3 As a sensitive material for acetone detection, there is generally a fast response and higher sensitivity, but a lower detection limit and a lower optimal temperature remain challenges.
The addition of other dopants also has a large impact on its gas-sensing properties. Doping affects sensing performance by creating lattice defects, oxygen vacancies, and grain size reduction in the sensing material. Different from other dopants, the noble metal has a special electronic structure and chemical properties, which can reduce the activation energy of adsorption and reaction, influence the distribution of current carriers, and improve the transfer efficiency of electrons, thereby improving the gas-sensitive performance. Chen et al synthesized Pt-doped NiO nanofibers with a sensor pair of 50ppm C 2 H 6 The sensitivity of (2) was improved from 4.67 to 29.14(W.G.Chen, Q.ZHou, F.Wan, S.D.Peng, W.Zeng, Nanoscience and Nanotechnology Letters,5(2013) 1231-1236.). However, the influence of the addition of the dopant on the gas-sensitive performance is usually adjusted by the doping amount, and the precise holding of the doping amount has certain difficulty. How to do with alpha-Fe 2 O 3 The gas sensitive material is modified to improve the content of alpha-Fe 2 O 3 The gas-sensitive characteristics of the sensor; how to achieve high gas-sensitive performance by finding precise doping amountAnd (5) amplitude is increased.
Through the above analysis, the problems and defects of the prior art are as follows: existing based on alpha-Fe 2 O 3 The working temperature and the detection lower limit of the sensor are higher, so that effective detection of gas with lower concentration is difficult to realize; the amount of dopant added has certain difficulties.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an acetone sensor, a preparation method and a detection method.
The invention synthesizes an environment-friendly gas sensitive material by a simple hydrothermal method, and realizes the detection of high sensitivity, low detection lower limit and high humidity of acetone. The invention is realized in such a way that a preparation method of an acetone sensor comprises the following steps:
(1) the Pt-doped alpha-Fe is successfully prepared by a one-step chemical hydrothermal method by taking ferric nitrate as a metal salt, an isopropanol/glycerol mixed solution as a solvent and sodium salicylate as a surfactant 2 O 3 Mesoporous microspheres;
(2) the Pt-doped alpha-Fe is coated, assembled and welded according to the indirectly heated device process 2 O 3 And (4) preparing the sensor.
Further, the content of the chemical reagents is 0.3-0.5 g of ferric nitrate respectively; 30-45 mL of isopropanol/glycerol mixed solution; 0.6-1 g of sodium salicylate; 100 μ L of chloroplatinic acid solution.
Further, the Pt-doped alpha-Fe 2 O 3 The mesoporous microsphere material specifically comprises:
(1) dissolving ferric nitrate and sodium salicylate in an isopropanol/glycerol mixed solvent, and continuously stirring at room temperature for 30-60 min to form a uniform solution;
(2) transferring the uniformly dispersed solution into 50ml of a stainless steel autoclave lined with polytetrafluoroethylene, and heating the solution in an oven at 180 ℃ for 12 hours;
(3) after the hydrothermal reaction is finished, removing supernatant, transferring the precipitate into a centrifugal tube, and alternately centrifuging the precipitate for multiple times by using ethanol and deionized water respectively at the centrifugation speed of 6000-8000 rpm;
(4) then drying the centrifugal product in an oven at the temperature of 60-80 ℃;
(5) and finally, calcining the dried product in a muffle furnace at 200-400 ℃ for 1-3 h to obtain Pt-doped alpha-Fe 2 O 3 A material.
Further, the sensor preparation according to the indirectly heated device process specifically comprises:
(1) doping Pt with alpha-Fe 2 O 3 Grinding and mixing the mesoporous microsphere material powder and deionized water to form pasty slurry;
(2) uniformly coating the ground paste slurry on the outer surface of a ceramic tube by using a pen brush to form a thick gas-sensitive material film, wherein the ceramic tube is provided with a pair of gold electrodes and four platinum leads;
(3) baking the coated ceramic tube, and putting the ceramic tube into a muffle furnace for calcination after the gas-sensitive material film is completely dried;
(4) taking out the calcined ceramic tube, and enabling a nickel-chromium heating coil with the resistance value of 30-40 omega to penetrate through the ceramic tube to control the working temperature;
(5) welding and fixing the assembled ceramic tube on a hexagonal base through four platinum leads to finish the Pt-doping-based alpha-Fe 2 O 3 And (4) manufacturing the mesoporous microsphere sensor.
Further, the mixing mode of the materials and the deionized water is specifically as follows: first Pt-doped alpha-Fe 2 O 3 Putting the mesoporous microsphere material powder into a mortar, adding a proper amount of deionized water, grinding for 30s, and mixing to form pasty slurry; okra-like Co 3 O 4 The material powder and the deionized water are mixed according to the mass ratio of 2: 1-5: 1.
Further, uniformly coating the ground paste slurry on the outer surface of a ceramic tube by using a pen brush to form a gas-sensitive material film with the thickness of 8-20 microns, wherein the ceramic tube is provided with a pair of gold electrodes and four platinum leads; the ceramic tube has a length of 3.9 to 4.2mm, an inner diameter of 0.7 to 1.1 μm, and an outer diameter of 1.1 to 1.4 μm.
Further, baking the coated ceramic tube for 10-20 min, and after the gas sensitive material film is completely dried, putting the ceramic tube into a muffle furnace at 120-350 ℃ to calcine for 30-50 min.
Another object of the present invention is to provide an acetone sensor prepared by the method for preparing an acetone sensor, the acetone sensor comprising: a platinum lead, a gold electrode, a ceramic tube, a gas-sensitive material film, a nickel-chromium alloy heating coil and a hexagonal base; the ceramic tube is fixed on the hexagonal base by welding, the ceramic tube is provided with a pair of gold electrodes and four Pt leads, the gas sensitive material film is uniformly coated on the outer surface of the ceramic tube, and the nichrome heating coil penetrates through the inner side of the ceramic tube.
The invention also aims to provide a method for detecting acetone in an organic solvent, which uses the acetone sensor.
Another object of the present invention is to provide a method for detecting acetone in a chemical plant raw material, which uses the acetone sensor.
In combination with the technical solutions and the technical problems to be solved, please analyze the advantages and positive effects of the technical solutions to be protected in the present invention from the following aspects:
first, aiming at the technical problems existing in the prior art and the difficulty in solving the problems, the technical problems to be solved by the technical scheme of the present invention are closely combined with results, data and the like in the research and development process, and some creative technical effects are brought after the problems are solved. The specific description is as follows: the invention improves alpha-Fe by doping Pt 2 O 3 The sensitivity of the gas sensor and the test result show that the Pt-doped alpha-Fe prepared by the method is based on 2 O 3 The sensitivity of the sensor of the mesoporous microsphere material to 100ppm acetone gas at the optimal working temperature (175 ℃) is 105, and the effective detection of acetone can be realized. The invention successfully synthesizes the alpha-Fe by a one-step hydrothermal method 2 O 3 A gas sensitive material. The synthesis method is simple and the cost is low. The invention adopts a one-step hydrothermal method, takes sodium salicylate as a structure-directing agent, and changes PtThe doping content successfully realizes the great improvement of the gas-sensitive performance, and the synthesis method is simple and has low cost.
The method successfully prepares the alpha-Fe based on Pt doping 2 O 3 An acetone sensor of mesoporous microsphere material. The gas sensor has excellent gas-sensitive property to acetone gas, the sensitivity is 105, the optimal working temperature is 175 ℃, and the effective detection of acetone in low-temperature and high-humidity environment can be realized. And the synthesis process is simple.
The invention specifies the preparation of Pt-doped alpha-Fe 2 O 3 Mesoporous microsphere material parameter information: 0.3-0.5 g of ferric nitrate; 30-45 mL of isopropanol/glycerol mixed solution; 0.6-1 g of sodium salicylate; 100 μ L of chloroplatinic acid solution. Given preparation of alpha-Fe based on Pt doping 2 O 3 Acetone sensor parameter information of mesoporous microsphere material: pt doped alpha-Fe 2 O 3 The mass ratio of the mesoporous microsphere material powder to the deionized water is 2: 1-5: 1, and the grinding time is 30 s. Through the experimental conditions, the Pt doping-based alpha-Fe is completed 2 O 3 And (3) manufacturing an acetone sensor made of the mesoporous microsphere material.
The Pt-doped alpha-Fe is successfully prepared by the method 2 O 3 A mesoporous microsphere material. Pt-doped-based alpha-Fe prepared by using method of the invention 2 O 3 The acetone sensor of the mesoporous microsphere material has excellent sensing characteristics on acetone gas, the sensitivity is 105, the optimal working temperature is 175 ℃, and the acetone can be effectively detected in a low-temperature and high-humidity environment. The invention synthesizes Pt-doped alpha-Fe with high catalytic activity, high specific surface area, easy-to-diffuse channel, multiple active sites and high carrier concentration by using a simple process (one-step hydrothermal method) 2 O 3 A mesoporous microsphere material. Pt-doped alpha-Fe-based catalyst prepared by the invention 2 O 3 The acetone sensor of the mesoporous microsphere material can realize effective detection of acetone at a low working temperature of 175 ℃, and the sensitivity is 105. The gas sensor device prepared by the invention is an indirectly heated device, and has low cost and small volume.
Secondly, considering the technical scheme as a whole or from the perspective of products, the technical effect and advantages of the technical scheme to be protected by the invention are specifically described as follows: the lower detection limit of the invention is an important index for measuring the performance of the gas sensor. The gas sensor with the lower detection lower limit can effectively realize the detection of gas with lower concentration. Therefore, it is required to produce a gas sensor having high sensitivity. The addition of the dopant is beneficial to increasing the specific surface area of the product, improving the diffusion speed of gas molecules, providing a high-efficiency reaction field for the adsorption oxidation reaction of gas, and further realizing the improvement of the gas-sensitive performance. However, the currently reported improved synthesis process is complex, is not beneficial to wide application, and needs to be improved.
Third, as an inventive supplementary proof of the claims of the present invention, there are also presented several important aspects:
the expected income and commercial value after the technical scheme of the invention is converted are as follows: can realize the non-invasive detection of diabetes.
The technical scheme of the invention solves the technical problem that people are eagerly to solve but can not be successfully solved all the time: the detection of high humidity and low concentration of acetone gas at lower temperature is realized, and the sensitivity to 20ppb acetone is 1.24 at lower working temperature (175 ℃).
Drawings
FIG. 1 is a flow chart of a method for preparing an acetone sensor according to an embodiment of the present invention;
FIG. 2 shows α -Fe provided in the examples of the present invention 2 O 3 Scanning electron micrograph of the mesoporous microsphere undoped Pt and Pt doped material;
FIG. 3 is a Pt doped α -Fe provided by an embodiment of the present invention 2 O 3 An X-ray diffraction pattern of the mesoporous microsphere material;
FIG. 4 shows Pt-based doped α -Fe according to an embodiment of the present invention 2 O 3 The schematic diagram of the curve of the response of the acetone sensor of the mesoporous microsphere material to 100ppm acetone along with the temperature change;
FIG. 5 shows Pt-based doped α -Fe according to an embodiment of the present invention 2 O 3 Acetone sensor of mesoporous microsphere materialSchematic diagram of the cycle induction transient curve for 100ppm acetone at the optimum working temperature (175 ℃);
FIG. 6 shows Pt-based doped α -Fe according to an embodiment of the present invention 2 O 3 The acetone sensor of the mesoporous microsphere material has a response value to various gases of 100ppm at the optimal working temperature (175 ℃);
FIG. 7 shows Pt-doped α -Fe with acetone gas according to an embodiment of the present invention 2 O 3 The structure schematic diagram of the gas sensor;
in the figure: 1. a platinum lead wire; 2. a gold electrode; 3. a ceramic tube; 4. a gas sensitive material layer; 5. a nichrome heating coil; 6. a hexagonal base.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
First, an embodiment is explained. This section is an explanatory embodiment expanding on the claims so as to fully understand how the present invention is embodied by those skilled in the art.
As shown in fig. 1, a method for preparing an acetone sensor provided by the embodiment of the present invention includes the following steps:
s101: ferric nitrate is used as metal salt, isopropanol/glycerol mixed solution is used as a solvent, sodium salicylate is used as a surfactant, a proper amount of noble metal Pt is added, and the Pt-doped alpha-Fe is successfully prepared by a one-step chemical hydrothermal method 2 O 3 Mesoporous microspheres;
s102: the Pt-doped alpha-Fe is coated, assembled and welded according to the indirectly heated device process 2 O 3 And (4) manufacturing the mesoporous microsphere sensor.
Pt doped alpha-Fe of the invention 2 O 3 The content of chemical reagents in the preparation process of the mesoporous microsphere gas-sensitive material is 0.3-0.5 g of ferric nitrate respectively; 30-45 mL of isopropanol/glycerol mixed solution; 0.6-1 g of sodium salicylate; 100 μ L of chloroplatinic acid solution.
The method for preparing the acetone sensor provided by the invention can be implemented by other steps by persons skilled in the art, and the method for preparing the acetone sensor provided by the invention in fig. 1 is only one specific example.
The Pt doped alpha-Fe provided by the embodiment of the invention 2 O 3 The specific preparation method of the mesoporous microsphere material comprises the following steps:
(1) dissolving ferric nitrate and sodium salicylate in an isopropanol/glycerol mixed solvent, and continuously stirring at room temperature for 30-60 min to form a uniform solution;
(2) transferring the uniformly dispersed solution into a stainless steel autoclave (50ml) lined with polytetrafluoroethylene, and heating in an oven at 180 ℃ for 12 hours;
(3) after the hydrothermal reaction is finished, removing supernatant, transferring the precipitate into a centrifugal tube, and alternately centrifuging the precipitate for multiple times by using ethanol and deionized water respectively at the centrifugation speed of 6000-8000 rpm;
(4) then drying the centrifugal product in an oven at the temperature of 60-80 ℃;
(5) and finally, calcining the dried product in a muffle furnace at 200-400 ℃ for 1-3 h to obtain Pt-doped alpha-Fe 2 O 3 A material.
The Pt doping-based alpha-Fe is completed according to the indirectly heated device process provided by the embodiment of the invention 2 O 3 The preparation method of the sensor specifically comprises the following steps:
(1) doping of Pt with alpha-Fe 2 O 3 Grinding and mixing the mesoporous microsphere material powder and deionized water to form pasty slurry;
(2) uniformly coating the ground paste slurry on the outer surface of a ceramic tube by using a pen brush to form a thick gas-sensitive material film, wherein the ceramic tube is provided with a pair of gold electrodes and four platinum leads;
(3) baking the coated ceramic tube, and putting the ceramic tube into a muffle furnace for calcination after the gas-sensitive material film is completely dried;
(4) taking out the calcined ceramic tube, and enabling a nickel-chromium heating coil with the resistance value of 30-40 omega to penetrate through the ceramic tube to control the working temperature;
(5) welding and fixing the assembled ceramic tube on a hexagonal base through four platinum leads to finish the Pt-doping-based alpha-Fe 2 O 3 And (4) manufacturing the mesoporous microsphere sensor.
The grinding and mixing mode of the material and the deionized water is as follows: first Pt-doped alpha-Fe 2 O 3 Putting the mesoporous microsphere material powder into a mortar, adding a proper amount of deionized water, grinding for 30s, and mixing to form pasty slurry. Pt doped alpha-Fe 2 O 3 The mass ratio of the mesoporous microsphere material powder to the deionized water is 2: 1-5: 1.
After testing, the Pt-doped based alpha-Fe prepared by the method of the invention 2 O 3 The acetone sensor of the mesoporous microsphere material has excellent sensing characteristics on acetone gas, the sensitivity is 105, the optimal working temperature is 175 ℃, and effective detection on acetone in low-temperature and high-humidity environments can be realized.
Based on Pt-doped alpha-Fe in the invention 2 O 3 The working mechanism of the material acetone sensor is that when the prepared sensor is in different environments, the resistance value changes correspondingly. For example: when the material is exposed to air, oxygen molecules absorb electrons from the material and adsorb on the surface of the material to form a high-density depletion layer, and the working resistance is high. When exposed to acetone, the adsorbed oxygen will react with acetone molecules to produce CO 2 、H 2 O, free electrons, the released free electrons return to the conduction band, resulting in an increase in electron density, at which point the operating resistance decreases.
As shown in FIG. 7, the invention provides Pt-based doped alpha-Fe 2 O 3 The mesoporous microsphere material acetone sensor device structure comprises: platinum lead 1, gold electrode 2, ceramic tube 3, gas sensitive material film 4, nichrome heating coil 5, hexagonal base 6. The ceramic tube 3 is fixed on the hexagonal base 6 through welding, the ceramic tube 3 is provided with a pair of gold electrodes 2 and four Pt lead wires 1, the outer surface of the ceramic tube 3 is uniformly coated with a gas sensitive material film 4, and a nichrome heating coil 5 penetrates through the inner side of the ceramic tube 3.
The technical solution of the present invention is further described with reference to the following specific examples.
The preparation method of the nickel cobaltate gas sensor provided by the invention comprises the following steps:
(1) 0.3-0.5 g of ferric nitrate, 30-45 mL of isopropanol/glycerin mixed solution, 0.6-1 g of sodium salicylate and 600 mu L of chloroplatinic acid solution are stirred at room temperature for 15-40 min to form a uniform solution. The uniformly dispersed solution was transferred to a stainless steel autoclave (50ml) lined with polytetrafluoroethylene and heated in an oven at 180 ℃ for 12 hours. And (5) after the hydrothermal time is over, removing the supernatant, and transferring the precipitate into a centrifugal tube. The precipitate was subjected to alternate centrifugation with ethanol and deionized water, respectively, at a centrifugation speed of 6000-. And then drying the centrifugal product in an oven at the temperature of 60-80 ℃. And finally, calcining the dried product in a muffle furnace at 200-500 ℃ for 1-3 h to obtain Pt-doped alpha-Fe 2 O 3 A mesoporous microsphere material. The scanning picture is shown in figure 2.
(2) Doping of Pt with alpha-Fe 2 O 3 Putting the mesoporous microsphere material powder into a mortar, adding a proper amount of deionized water and Pt-doped alpha-Fe 2 O 3 Grinding and mixing mesoporous microsphere material powder and deionized water for 30 seconds to form pasty slurry, wherein the mass ratio of the mesoporous microsphere material powder to the deionized water is 2: 1-5: 1;
(3) taking a small amount of fully ground paste slurry, and uniformly coating the paste slurry on the outer surface of the ceramic tube by using a pen brush to form a gas-sensitive material film with the thickness of 8-20 microns. The ceramic tube has a pair of gold electrodes and four platinum leads. The length of the ceramic tube is 3.9-4.2 mm, the inner diameter is 0.7-1.1 μm, and the outer diameter is 1.1-1.4 μm;
(4) baking the coated ceramic tube for 10-20 min, and after the gas-sensitive material film is completely dried, putting the ceramic tube into a muffle furnace at 120-350 ℃ for calcining for 30-50 min;
(5) taking out the calcined ceramic tube, and enabling a nickel-chromium heating coil with the resistance value of 30-40 omega to penetrate through the ceramic tube to control the working temperature;
(6) and welding and fixing the assembled ceramic tube on the hexagonal base through four platinum leads to finish the preparation based on the okra-shaped sensor.
And II, application embodiment. In order to prove the creativity and the technical value of the technical scheme of the invention, the part is the application example of the technical scheme of the claims on specific products or related technologies.
The lowest detection concentration of acetone gas serving as an expiration marker of a diabetic patient needs to be less than 1.8ppm, the lowest detection lower limit of the gas sensor can reach 20ppb, and meanwhile, the sensor can effectively detect acetone with lower concentration under high humidity because the expiration contains a large amount of water vapor. Therefore, the kit can better assist in the detection of diabetes.
And thirdly, evidence of relevant effects of the embodiment. The embodiment of the invention achieves some positive effects in the process of research and development or use, and has great advantages compared with the prior art, and the following contents are described by combining data, diagrams and the like in the test process.
FIG. 2 is Pt doped α -Fe 2 O 3 The scanning electron micrograph of the mesoporous microsphere material shows that the prepared okra-shaped Ni-doped Co 3 O 4 The material has good dispersibility and obvious hierarchical structure.
FIG. 3 is Pt doped α -Fe 2 O 3 The X-ray diffraction pattern of the mesoporous microsphere material shows that the main body of the prepared gas-sensitive material is alpha-Fe 2 O 3 The corresponding standard card is PDF # 89-8103. After testing, it was found that Pt-doped based alpha-Fe prepared by the method of the present invention 2 O 3 The acetone sensor of the mesoporous microsphere material shows excellent sensing characteristics for acetone gas. The test results are shown in fig. 4, 5 and 6.
FIG. 4 shows Pt-based doped alpha-Fe of the present invention 2 O 3 The response of the acetone sensor of the mesoporous microsphere material to 100ppm acetone is plotted along with the change of temperature, and the response of the sensor to 100ppm acetone at 175 ℃ is up to 105.
FIG. 5 shows Pt-based doped α -Fe of the present invention 2 O 3 The acetone sensor of the mesoporous microsphere material can circularly sense a transient curve to 100ppm acetone at 175 ℃, and the sensor can be seen to have good repeatabilityAnd (4) the method is suitable for actual detection.
FIG. 6 shows Pt-based doped α -Fe of the present invention 2 O 3 The response value radar chart of the acetone sensor of the mesoporous microsphere material to various VOC gases of 100ppm at 175 ℃ shows that the sensor has good selectivity to acetone.
Given preparation of Pt-doped alpha-Fe 2 O 3 Mesoporous microsphere material parameter information: in the preparation process, the contents of the chemical reagents are 0.3-0.5 g of ferric nitrate, 30-45 mL of isopropanol/glycerol mixed solution, 0.6-1 g of sodium salicylate and 600 muL of chloroplatinic acid solution. Given preparation of alpha-Fe based on Pt doping 2 O 3 Acetone sensor parameter information of mesoporous microsphere material: pt doped alpha-Fe 2 O 3 The mass ratio of the mesoporous microsphere material powder to the deionized water is 2: 1-5: 1, and the grinding time is 30 s.
Through the experimental data, Pt-doped alpha-Fe is completed 2 O 3 The prepared gas sensor shows excellent sensing characteristics on acetone gas, the sensitivity is 105, the optimal working temperature is 175 ℃, and effective detection on acetone in low-temperature and high-humidity environments can be realized.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210309012.7A CN114813854A (en) | 2022-03-28 | 2022-03-28 | Acetone sensor, preparation method and detection method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210309012.7A CN114813854A (en) | 2022-03-28 | 2022-03-28 | Acetone sensor, preparation method and detection method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114813854A true CN114813854A (en) | 2022-07-29 |
Family
ID=82529911
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210309012.7A Pending CN114813854A (en) | 2022-03-28 | 2022-03-28 | Acetone sensor, preparation method and detection method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114813854A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105738421A (en) * | 2014-12-30 | 2016-07-06 | 通用电气公司 | Material and sensor for detecting gaseous agents |
| CN108802116A (en) * | 2018-06-19 | 2018-11-13 | 扬州睿德石油机械有限公司 | A kind of preparation method of acetone gas sensitive material |
| 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 |
| US20210104140A1 (en) * | 2016-12-09 | 2021-04-08 | Samsung Electronics Co., Ltd. | Electronic device and control method therefor |
| CN112666230A (en) * | 2020-12-29 | 2021-04-16 | 西安电子科技大学 | Acetone sensor, preparation method and acetone detection method |
-
2022
- 2022-03-28 CN CN202210309012.7A patent/CN114813854A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105738421A (en) * | 2014-12-30 | 2016-07-06 | 通用电气公司 | Material and sensor for detecting gaseous agents |
| US20210104140A1 (en) * | 2016-12-09 | 2021-04-08 | Samsung Electronics Co., Ltd. | Electronic device and control method therefor |
| CN108802116A (en) * | 2018-06-19 | 2018-11-13 | 扬州睿德石油机械有限公司 | A kind of preparation method of acetone gas sensitive material |
| 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 |
| CN112666230A (en) * | 2020-12-29 | 2021-04-16 | 西安电子科技大学 | Acetone sensor, preparation method and acetone detection method |
Non-Patent Citations (2)
| Title |
|---|
| BO ZHANG ET AL: "Enhanced gas sensing properties to acetone vapor achieved by α-Fe2O3 particles ameliorated with reduced graphene oxide sheets", SENSORS AND ACTUATORS B, vol. 241, 5 November 2016 (2016-11-05), pages 904 - 914, XP029864223, DOI: 10.1016/j.snb.2016.11.023 * |
| SHENDAN ZHANG ET AL: "An acetone gas sensor based on nanosized Pt-loaded Fe2O3 nanocubes", SENSORS AND ACTUATORS B: CHEMICAL, vol. 290, 28 March 2019 (2019-03-28), pages 59 - 67 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112666230A (en) | Acetone sensor, preparation method and acetone detection method | |
| Yang et al. | Highly selective and humidity-resistant triethylamine sensors based on Pt and Cr2O3 nanoparticles | |
| CN101419181A (en) | Air-sensitive material for detecting oxymethylene and air-sensitive device made from the material | |
| CN105628748A (en) | Platinum-loaded tin dioxide nanofiber gas-sensitive material and gas-sensitive element made from same | |
| CN109142465B (en) | Preparation method of cerium-doped tin dioxide sensing material for detecting formaldehyde at low temperature | |
| CN107064220B (en) | A kind of the zno-based acetylene sensor and preparation method of ultra-fine Au particle modification | |
| CN108956715B (en) | Au @ WO3Core-shell structure nanosphere and preparation method and application thereof | |
| CN106770497A (en) | One kind is based on Pt/ α Fe2O3Acetone gas sensor of porous nanoparticles sensitive material and preparation method thereof | |
| CN109001263A (en) | A method of the gas sensor based on MOF templated synthesis ZnO load di-iron trioxide nano-heterogeneous structure | |
| Ji et al. | Boosting acetone response of p-type Co3O4 sensor via Sn and Ni co-doping for diabetes diagnosis | |
| CN103399040B (en) | Gas-sensitive material for detecting acetaldehyde and method for producing gas-sensitive component by utilizing gas-sensitive material | |
| Wang et al. | Tailoring the Ni–O microenvironment in amorphous-dominated highly active and stable Zn/NiO for hydrogen sulfide detection | |
| Zheng et al. | Sandwich-type electrochemical immunosensor for carcinoembryonic antigen detection based on the cooperation of a gold–vertical graphene electrode and gold@ silica–methylene blue | |
| CN110068599B (en) | Based on CoFe2O4/Co3O4Formaldehyde gas sensor made of double-shell structure cubic material and preparation method thereof | |
| CN113899790A (en) | Acetone sensor, preparation method and application | |
| CN108956708A (en) | A kind of alcohol gas sensor and preparation method thereof based on zinc ferrite nano sensitive material | |
| Jin et al. | Dual functionalized Co3O4 porous cages with Pd and Co-MOF for acetone gas sensing under high humidity | |
| Hedau et al. | High-performance non-enzymatic electrochemical dopamine sensors based on metal-organic framework derived Co-C-matrix nanoplatforms | |
| CN109596676A (en) | Based on CexMn1-xO2-SnO2The gas sensor of material and its preparation and application | |
| CN113960122B (en) | Three-dimensional SnO2/Co3O4Core-shell nanocomposite and moisture-resistant acetone gas sensor prepared from same | |
| CN114813854A (en) | Acetone sensor, preparation method and detection method | |
| CN112694072A (en) | Fe-Ni metal nitride composite material, preparation method thereof and application thereof in glucose sensor | |
| Ding et al. | Synergistic integration of hierarchical structure and oxygen vacancy engineering in core-shelled Ni and Zn co-doped Co3O4 microsphere for efficient detection of triethylamine gas: W. Ding et al. | |
| CN108152337A (en) | A kind of LaFeO of high air-sensitive property energy3Base alcohol gas sensor and preparation method thereof | |
| CN111551592A (en) | NiO/Zn based on octahedral structure2SnO4Acetone gas sensor of composite sensitive material and preparation method thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220729 |