CN112255279A - Flower-shaped V2O5Preparation of microsphere and application of microsphere in acetone gas sensor - Google Patents
Flower-shaped V2O5Preparation of microsphere and application of microsphere in acetone gas sensor Download PDFInfo
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- CN112255279A CN112255279A CN202011050513.5A CN202011050513A CN112255279A CN 112255279 A CN112255279 A CN 112255279A CN 202011050513 A CN202011050513 A CN 202011050513A CN 112255279 A CN112255279 A CN 112255279A
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- 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
Abstract
Flower-shaped V2O5The invention discloses a preparation of microspheres and application thereof in an acetone gas sensor, relates to the preparation of metal oxide and the application of the gas sensor, and adopts a hydrothermal synthesis method and NH4VO3Is a vanadium source, PVP and citric acid are used as regulators, and V with a shape microsphere structure with good appearance structure is synthesized in situ on the surface of the ceramic chip substrate2O5. The gas sensor prepared by the production process can effectively avoid the defects of falling of sensitive materials in the using process, poor device stability and the like, and the whole production process has low cost and simple and easy operation and is suitable for large-scale production. The flower-like microsphere structure V is prepared by the method2O5The sensor has the advantages of high porosity, increased specific surface area of the material, favorable adsorption and desorption of gas, good sensitivity in acetone gas detection, high sensitivity, quick response-recovery time, good stability and the like, and meanwhile, the sensor element has small volume and simple process, and is suitable for being used as a sensor elementThe method has wide application prospect in the field of preparing integrated high-performance gas sensors by mass production.
Description
Technical Field
The invention relates to preparation of metal oxide and application of a gas sensor, in particular to a flower-shaped V2O5Preparation of microspheres and application thereof in an acetone gas sensor.
Background
V2O5The material is a common semiconductor material, and has been widely researched in various fields due to its special layered structure, variable valence state and its unique properties in the aspects of electricity, optics, physical chemistry and the like. At present, V2O5The material has been widely used in the fields of lithium ion batteries, capacitors, antistatic coatings, voltage switches, electrochromic display devices, and the like. In recent years, V2O5Because of its unique structure and photochromic characteristic, it is receiving more and more attention from people in the research aspect of gas sensor. V with various structures and shapes for meeting the development requirement of gas detection2O5Nanomaterials, e.g. nanoparticles, nanobelts, nanoneedles, nanoblocks, V2O5Thin films were prepared and used for gas sensor research. In a plurality of V2O5In the nano/micro structure, V2O5The hierarchical porous structure has the structural and functional advantages of large specific surface area, high porosity, good permeability, good agglomeration resistance and the like, so that the hierarchical porous structure has good application prospect in the field of gas sensors. Thus, a simple and controllable process was developed to design and prepare V2O5The device has a hierarchical structure, and has very important significance in monitoring various toxic and harmful gases in the environment.
From the viewpoint of environmental protection and human safety, rapid detection and identification methods of volatile organic compounds have become a current research hotspot. Acetone is widely used as a solvent, a chemical intermediate and an industrial product in industry and laboratories, but as a toxic volatile gas, it can enter the human body through the respiratory and digestive systems of the skin, causing great harm to the human body. Furthermore, with the recent development of nondestructive medical diagnosis, the use of gas sensors to detect the concentration of certain specific exhalation markers has become an important means for achieving non-invasive, real-time, inexpensive diagnosis and early prevention of diseases. Acetone is a specific biomarker gas in the exhaled gas of diabetes, can be analyzed through the content of acetone in the exhaled gas of a patient, so that noninvasive diagnosis of diabetes is realized, and the acetone is applied to daily physical examination of people and becomes more real-time and effective. Currently, many methods for detecting and analyzing acetone have been developed, and gas chromatography is the main method for rapid and accurate measurement. However, the instrumentation required in this process is expensive and complex, and is not convenient for rapid real-time detection and analysis of acetone. Therefore, the acetone gas sensor with high sensitivity, good selectivity and good stability is developed, and powerful technical support can be provided for the aspects of intelligent safety, intelligent environmental protection, intelligent medical treatment and healthy home construction in China.
Disclosure of Invention
The invention aims to provide a flower-shaped V2O5The invention discloses a preparation method of microspheres and application thereof in an acetone gas sensor2O5The microsphere is prepared into a gas sensor for detecting acetone gas.
The purpose of the invention is realized by the following technical scheme:
flower-like microsphere structure V grown on surface of ceramic wafer electrode in situ2O5The method has the following processes and steps:
(1) (the alumina ceramic substrate is respectively put into acetone, absolute ethyl alcohol and deionized water for 10 minutes of ultrasonic treatment, and the surface impurities are cleaned;
(2) taking NH by balance4VO3PVP is dissolved in 15 mL of deionized water, and the solution is magnetically stirred for about 10 minutes at room temperature; dissolving citric acid in 5 mL of deionized water until the citric acid is dissolved, pouring the solution into the deionized water, and stirring the solution at normal temperature for about 20 minutes until the solution is light yellow to prepare a hydrothermal synthesis precursor solution;
(3) pouring the hydrothermal synthesis precursor solution into a high-pressure reaction kettle with a polytetrafluoroethylene stainless steel lining, placing the cleaned ceramic chip electrode into the reaction solution, and sealing; preserving heat for 1-16 hours at 180 ℃, and then cooling to room temperature along with the furnace to obtain a product;
(4) repeatedly washing the surface of the ceramic wafer electrode by using distilled water and absolute ethyl alcohol respectively to remove impurities;
(5) putting the washed ceramic chip electrode with the product into a constant-temperature blast drying box, and drying at 60 ℃ for 12 hours;
(6) putting the dried ceramic wafer electrode into a clean crucible, putting the crucible into a muffle furnace, and calcining for 2 hours at 400 ℃ to obtain the ceramic wafer with V attached to the surface2O5Yellow powder product, which is stored in a desiccator to be assayed.
In-situ growth flower-shaped microsphere structure V on surface of ceramic wafer electrode2O5The application of (1) and the preparation method of the acetone gas sensor are as follows:
(1) respectively welding four lead wires of the ceramic plate electrode on a four-pin base to obtain a gas sensor;
(2) placing the prepared gas sensor on an aging table, aging for 2 days at 450 ℃ in an air environment to obtain the flower-shaped V-based gas sensor2O5Microsphere acetone gas sensors.
The invention has the advantages and effects that:
(1) the invention grows flower-shaped V on the surface of the ceramic chip electrode in situ by a hydrothermal synthesis technology2O5The microsphere has the advantages of low cost, good controllability, high purity of prepared materials and good crystallization, improves the adhesion of the sensitive film on the surface of the substrate, effectively avoids the problem of falling and damage of the sensitive film, reduces Schottky barrier of contact between a semiconductor material and an electrode, improves the stability of the sensor, is suitable for batch production of devices, and has wide application prospect in the aspect of manufacturing gas sensors.
(2) Flower-shaped V prepared by the invention2O5The microsphere has a unique spatial structure, a large specific surface area and developed hierarchical pore channels, so that the adsorption and desorption capacity of target gas is increased, the material can be ensured to have good structural stability, and the microsphere shows good detection characteristics on acetone gas.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of the product prepared in the example;
FIG. 2 is a scanning electron micrograph of a product prepared in example;
FIG. 3(a) is a graph showing the sensitivity of the gas sensor to 5 ppm acetone gas as a function of operating temperature for the example and a physical diagram of a gas sensor element prepared according to the present invention;
FIG. 3(b) is a graph of time response versus recovery for various concentrations of acetone gas at 300 ℃ for the sensor of example 1;
FIG. 3(c) is a graph of the sensitivity of the sensor of example 1 to acetone gas concentration at 300 ℃;
FIG. 3(d) is a graph showing the sensitivity of the sensor of example 1 to 5 ppm of different organic volatile gases at 300 ℃.
Detailed Description
The present invention will be described in detail with reference to the embodiments shown in the drawings.
Flower shape V of the invention2O5The raw materials required for preparing the microsphere structure are as follows: ammonium metavanadate (NH)4VO3) Polyvinyl pyrrolidone (PVP) and citric acid through washing, drying and calcining. Prepared flower-shaped V2O5The diameter of the microsphere is 5-10 um, and the gas sensor has higher sensitivity, quick response-recovery characteristic and good selectivity to acetone.
(1) The flower shape V2O5The preparation method of the microsphere comprises the following steps:
the method comprises the following steps: and (3) respectively carrying out ultrasonic treatment on the aluminum oxide ceramic wafer in acetone, absolute ethyl alcohol and deionized water for 10 minutes, and cleaning surface impurities.
Step two: firstly, a certain amount of NH is taken by balance4VO3PVP is dissolved in 15 mL of deionized water, and the solution is magnetically stirred for about 10 minutes at room temperature; and dissolving a certain amount of citric acid in 5 mL of deionized water until the citric acid is dissolved, pouring the solution into the solution, and stirring the solution for about 20 minutes at normal temperature until the solution is light yellow to prepare a hydrothermal synthesis precursor solution.
Step three: and (3) pouring the precursor solution obtained in the first step into a polytetrafluoroethylene stainless steel lined high-pressure reaction kettle, wherein the filling degree is 80%. And (4) placing the cleaned ceramic wafer electrode in the reaction solution, and sealing. Preserving the heat for 1 to 16 hours at 180 ℃, and then cooling to room temperature along with the furnace to obtain the product.
Step four: and (4) washing the ceramic wafer reacted in the step three with absolute ethyl alcohol and distilled water for 3 times in sequence.
Step five: and (4) putting the ceramic chip electrode obtained in the step four into a constant-temperature blast drying box, and drying at 60 ℃ for 12 hours. Putting the dried product into a clean crucible, putting the crucible into a muffle furnace, and calcining for 2 hours at 400 ℃ to obtain the ceramic tube with V attached to the surface2O5Yellow powder product, which is stored in a desiccator to be assayed.
(2) The utilization surface is attached with V2O5Preparing a gas sensor by using the yellow powder ceramic chip electrode:
the method comprises the following steps: and respectively welding four lead wires of the ceramic wafer electrode on the four-pin base to obtain the gas sensor.
Step two: placing the prepared gas sensor on an aging table, aging for 2 days at 450 ℃ in an air environment to obtain the flower-shaped V-based gas sensor2O5Microsphere acetone gas sensors. .
Step three: and a WS-30A gas-sensitive tester is adopted to test the gas sensitivity characteristic of the sensor. The test temperature was 100-400 ℃.
Detailed description of the preferred embodiment 1
(1) In-situ growth of flower-shaped V on the surface of ceramic wafer electrode2O5Microsphere preparation:
the method comprises the following steps: and (3) respectively carrying out ultrasonic treatment on the aluminum oxide ceramic wafer in acetone, absolute ethyl alcohol and deionized water for 10 minutes, and cleaning surface impurities.
Step two: 0.117 g NH4VO30.1125 g of PVP is dissolved in 15 mL of deionized water and magnetically stirred at room temperature for about 10 minutes; dissolving 0.315 g of citric acid in 5 mL of deionized water until the citric acid is dissolved, pouring the solution into the solution, stirring the solution at normal temperature for about 20 minutes until the solution is light yellow, and preparing the solution before hydrothermal synthesisAnd (4) expelling liquid.
Step three: and pouring the precursor liquid in the step two into a polytetrafluoroethylene stainless steel lined high-pressure reaction kettle, wherein the filling degree is 80%. And (4) placing the cleaned ceramic wafer electrode in the reaction solution, and sealing. Keeping the temperature at 180 ℃ for 12 hours, then cooling to room temperature along with the furnace, and obtaining the product on the surface of the ceramic chip.
Step four: and (4) washing the ceramic wafer reacted in the step three with absolute ethyl alcohol and distilled water for 3 times in sequence.
Step five: and (4) putting the ceramic chip electrode obtained in the step four into a constant-temperature blast drying box, and drying at 60 ℃ for 12 hours. Putting the dried product into a clean crucible, putting the crucible into a muffle furnace, and calcining for 2 hours at 400 ℃ to obtain the ceramic plate with V attached to the surface2O5Yellow powder product, which is stored in a desiccator to be assayed.
(2) Flower shape V2O5Structural characterization of microspheres
The crystal structure of the product was characterized using an XRD powder diffractometer (XRD, PANALYTICAL X' Pert Pro). As shown in FIG. 1, the diffraction characteristic peaks are all strong, and no other impurity peaks appear, indicating that the prepared sample has good crystallinity and purity. The diffraction peak completely accords with NO.41-1426 in the standard PDF card, so that the sample has an orthogonal phase V2O5。
The morphology of the product was characterized by scanning electron microscopy (FESEM, ZEISS Ultra Plus). As shown in fig. 2(a), a layer of uniform product is attached to the surface of the ceramic tube, and the morphology of the product is flower-like microspheres in the form of nano-sheet groups, so that the product has excellent dispersibility and uniformity. The thickness of the nano-sheets forming the flower-shaped microspheres is about 20 nm, the diameter of the microspheres is 1-5 μm, and a plurality of gaps exist among the nano-sheet structures, so that the flower-shaped microspheres play an important role in improving trimethylamine detection.
Example 2
(1) In-situ growth of flower-shaped V on the surface of ceramic wafer electrode2O5Microsphere preparation:
the first step and the second step are the same as those in the example 1.
Step three: and (5) placing the reaction kettle in the second step into an oven, preserving the heat for 1 hour at the temperature of 180 ℃, and then cooling.
It was found that no product was deposited on the ceramic wafer surface within 1 hour of incubation, indicating that too short a reaction time is detrimental to the growth of product on the ceramic wafer surface.
Example 3
(1) In-situ growth of flower-shaped V on the surface of ceramic wafer electrode2O5Microsphere preparation:
the first step and the second step are the same as those in the example 1.
Step three: and (5) placing the reaction kettle in the second step into an oven, preserving the heat for 4 hours at the temperature of 180 ℃, and then cooling.
The fourth and fifth steps are the same as example 1.
(2) Flower shape V2O5Structural characterization of microspheres
The crystal structure of the product was characterized by XRD powder diffractometer. As can be seen from FIG. 1, all diffraction characteristic peaks of the product completely correspond to No.41-1426 of the standard PDF card, so that the sample has an orthogonal phase V2O5. And characterizing the morphology of the product by adopting a scanning electron microscope. As shown in FIG. 2(b), the product was aggregated from irregular nano-agglomerates with a diameter of 100-200 nm, and some aggregates showed a microsphere structure.
Example 4
(1) In-situ growth of flower-shaped V on the surface of ceramic wafer electrode2O5Microsphere preparation:
the first step and the second step are the same as those in the example 1.
Step three: and (5) placing the reaction kettle in the second step into an oven, preserving the heat for 8 hours at the temperature of 180 ℃, and then cooling.
The fourth and fifth steps are the same as example 1.
(2) Flower shape V2O5Structural characterization of microspheres
The crystal structure of the product was characterized by XRD powder diffractometer. As can be seen from FIG. 1, all diffraction characteristic peaks of the product completely correspond to No.41-1426 of the standard PDF card, so that the sample has an orthogonal phase V2O5. And characterizing the morphology of the product by adopting a scanning electron microscope. As shown in FIG. 2(c)The product is a flower-shaped morphology structure assembled by nano sheets, and the diameter is between 300 and 500 nm.
Example 5
(1) In-situ growth of flower-shaped V on the surface of ceramic wafer electrode2O5Microsphere preparation:
the first step and the second step are the same as those in the example 1.
Step three: and (5) placing the reaction kettle in the second step into an oven, preserving the heat for 16 hours at the temperature of 180 ℃, and then cooling.
The fourth and fifth steps are the same as example 1.
(2) Flower shape V2O5Structural characterization of microspheres
The crystal structure of the product was characterized by XRD powder diffractometer. As can be seen from FIG. 1, all diffraction characteristic peaks of the product completely correspond to No.41-1426 of the standard PDF card, so that the sample has an orthogonal phase V2O5. And characterizing the morphology of the product by adopting a scanning electron microscope. As shown in fig. 2(d), the product is microspherical and slightly varied in morphology, with some flower-like structures broken and some irregular nanoparticles appearing.
Flower-like V made by the example2O5The microspheres are prepared into a gas sensor, and the gas-sensitive performance of acetone gas is tested:
attaching V to the surface2O5The yellow powder ceramic plate electrode was welded on a four-pin base and aged on an aging table for 24 hours to produce a gas sensor element, as shown in fig. 3 (a). And a WS-30A gas-sensitive tester is adopted to test the gas sensitivity characteristic of the sensor.
FIG. 3(a) is a graph showing the sensitivity of the prepared sensor to 5 ppm acetone gas at a temperature of 150 ℃ and 400 ℃. It can be seen from the graph that the sensor prepared in example 1 has the highest sensitivity, reaching 2.17 at 300 ℃, which is higher than the sensors prepared in other examples. Thus, flower-like V is obtained with a reaction time of 12 h2O5The microsphere is the best gas sensor material for detecting acetone gas. For real-time efficient detection of target gases, responses andrecovery characteristics are an important measure of gas sensor performance. FIG. 3(b) is a graph showing the response-recovery curve of the sensor prepared in example 1 at 300 ℃ for 1-100 ppm acetone gas. As can be seen from the graph, the resistance dropped sharply when the sensor was exposed to acetone gas, and then returned to its initial value after acetone gas was released, indicating that they had rapid and reversible response and recovery characteristics. As can be seen from the corresponding concentration sensitivity relationship (fig. 3 (c)), when the acetone gas concentration is lower than 50 ppm, the sensor rapidly increases in sensitivity up to 50 ppm as the gas concentration increases. The upward trend of the response gradually slowed down at concentrations of 50-100 ppm, indicating that the sensor gradually tended to saturate. The sensor prepared in the example 1 can detect acetone gas in a wider range (1-100 ppm), and particularly the detection characteristics of the sensor at low concentration can realize accurate detection of acetone gas in the fields of environment, medical treatment and the like. The response characteristics of the sensor prepared in example 4 at 300 deg.C for several volatile gases at 5 ppm are shown in FIG. 3 (d). As can be seen from the figure, the sensitivity of the sensor to acetone is the highest, and is more than twice of that of other gases, which shows that the sensor can selectively detect acetone gas.
Claims (2)
1. Flower-like microsphere structure V grown on surface of ceramic wafer electrode in situ2O5Characterized in that the method comprises the following steps:
(1) respectively carrying out ultrasonic treatment on the alumina ceramic substrate in acetone, absolute ethyl alcohol and deionized water for 10 minutes, and cleaning surface impurities;
(2) taking NH by balance4VO3PVP is dissolved in 15 mL of deionized water, and the solution is magnetically stirred for about 10 minutes at room temperature; dissolving citric acid in 5 mL of deionized water until the citric acid is dissolved, pouring the solution into the deionized water, and stirring the solution at normal temperature for about 20 minutes until the solution is light yellow to prepare a hydrothermal synthesis precursor solution;
(3) pouring the hydrothermal synthesis precursor solution into a high-pressure reaction kettle with a polytetrafluoroethylene stainless steel lining, placing the cleaned ceramic chip electrode into the reaction solution, and sealing; preserving heat for 1-16 hours at 180 ℃, and then cooling to room temperature along with the furnace to obtain a product;
(4) repeatedly washing the surface of the ceramic wafer electrode by using distilled water and absolute ethyl alcohol respectively to remove impurities;
(5) putting the washed ceramic chip electrode with the product into a constant-temperature blast drying box, and drying at 60 ℃ for 12 hours;
(6) putting the dried ceramic wafer electrode into a clean crucible, putting the crucible into a muffle furnace, and calcining for 2 hours at 400 ℃ to obtain the ceramic wafer with V attached to the surface2O5Yellow powder product, which is stored in a desiccator to be assayed.
2. In-situ growth flower-shaped microsphere structure V on surface of ceramic wafer electrode2O5The application is characterized in that the acetone gas sensor is manufactured by the following method:
(1) respectively welding four lead wires of the ceramic plate electrode on a four-pin base to obtain a gas sensor;
(2) placing the prepared gas sensor on an aging table, aging for 2 days at 450 ℃ in an air environment to obtain the flower-shaped V-based gas sensor2O5Microsphere acetone gas sensors.
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| WO2023207282A1 (en) * | 2022-04-25 | 2023-11-02 | 广东邦普循环科技有限公司 | Template growth method for preparing lithium cobaltate precursor and use thereof |
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