CN113406155B - Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof - Google Patents
Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof Download PDFInfo
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- CN113406155B CN113406155B CN202110695696.4A CN202110695696A CN113406155B CN 113406155 B CN113406155 B CN 113406155B CN 202110695696 A CN202110695696 A CN 202110695696A CN 113406155 B CN113406155 B CN 113406155B
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- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention provides a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and a preparation method thereof. The material main body is three layers of coaxial nanofiber materials, a core layer is tin oxide, a middle layer is polyacid, a shell layer is tungsten oxide, and the three substances are distributed in a three-layer cable shape. The existence of gas such as ethanol in the air can be detected by utilizing the change of an electrochemical signal at a certain working temperature. The material is prepared by combining a coaxial electrostatic spinning method with oxidation calcination, has simple method and low cost, can effectively detect gases such as ethanol with low concentration in the air, and is suitable for development and production of a polyacid type high-performance gas sensor.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and relates to a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and a preparation method thereof.
Background
Ethanol, commonly known as ethanol, is an organic substance, of formula C 2 H 6 O, ethanol is a flammable, volatile, colorless and transparent liquid at normal temperature and pressure. The ethanol vapor can form an explosive mixture with air and can be mutually soluble with water in any proportion. The ethanol has wide application range, and can be used for preparing acetic acid, beverages, essence, fuels, fuel and the like. In medical treatment, 70-75% volume fraction ethanol is also commonly used as a disinfectant, and has wide application in national defense chemical industry, medical treatment and health, food industry, industrial and agricultural production. Because ethanol is volatile, the vapor and air can form explosive mixture, and the explosion is easily caused by the exposure to open fire and high heat energyAnd (6) frying. Contact with the oxidant causes a chemical reaction or combustion. The ethanol gas can easily enter human body through inhalation, ingestion, percutaneous absorption and other ways. The human body inhales excessive ethanol to cause life risks such as loss of consciousness, dilated pupils, irregular breathing, shock, heart circulation failure, respiratory arrest and the like; more serious patients may cause polyneuropathy, chronic gastritis, fatty liver, liver cirrhosis, myocardial damage, and organic psychosis. Prolonged contact with the skin can cause dryness, desquamation, chapping and dermatitis. Based on the above analysis, it is important to detect ethanol gas.
A gas sensor is a device that can convert certain information of a gas, including concentration and species, into data information that can be utilized. The physical and chemical properties of various gases are used to convert the change of the monitored gas into electric signals which can be easily processed, so that people can control and apply the gas correctly and effectively. Is the first link for realizing automatic detection and automatic control. The semiconductor material is one of the cores of the gas sensor, and has high sensitivity and simple operation. The practical application of the gas sensitive material with low cost and high performance is realized, and the development of a novel semiconductor material is urgently needed. So far, over half a century of research, tens of gas sensitive materials have been successively developed, developed and applied. However, the research focus is still on metal oxide semiconductors, wherein SnO 2 、ZnO、TiO 2 、WO 3 、In 2 O 3 And alpha-Fe 2 O 3 The n-type semiconductor material occupies more than 90% of the research field of gas sensing. However, the single-component semiconductor material has a high carrier recombination rate, which limits the performance of the gas-sensitive material. This also becomes a scientific problem limiting the development of gas sensitive materials. With the continuous and deep research of semiconductor gas sensors, people find that the gas-sensitive performance of semiconductor materials can be obviously improved by constructing a reasonable heterojunction. In the material of the zero-dimensional nanoparticles, at the grain boundaries, a large amount of recombination of electron and hole pairs can occur due to the presence of defects; at the same time, there are long carrier migration paths with random directions, which limit the gas-sensitive performance of the material. And a one-dimensional junctionThe materials such as the nano tube, the nano rod and the nano fiber can provide a preferential directional migration path for current carriers, and effectively promote the separation of electrons and holes, thereby improving the photoelectric performance of the materials.
Polyoxometalates (i.e. polyacids, Polyoxometalates, POMs) are polynuclear complexes, have a history of development for nearly two hundred years so far, and have become an important research field in inorganic chemistry. In recent years, polyacid has been studied in gas sensing. In 2011, Suzhong professor combined ascorbic acid with silicotungstic acid, which showed a significant color change in the presence of ammonia. In 2013, Khan and the like prepare polyvanadate with a frame structure, and have certain electrochemical response to the existence of nitrogen oxides. Respectively introducing polyacid into SnO by professor of Shanxi university in northeast China 2 、BiVO 3 And TiO 2 In addition, the sensor has sensing function on gases such as formaldehyde, toluene and the like. In addition, polyoxometallate (polyacid for short) is a good electron acceptor, and can inhibit the recombination of photon-generated carriers and promote the migration of the photon-generated carriers by capturing photon-generated electrons of a semiconductor conduction band, thereby being beneficial to electron transfer. However, in previous studies, the electron acceptor properties of polyacids have been mainly exploited to introduce polyacids into SnO in a simple molecularly doped form 2 And the like, in order to improve the gas-sensitive performance of the original semiconductor. The polyacid in the semiconductor material has low content, plays a main role in the original semiconductor material, is in a disordered state, is distributed on the surface and bulk phase of the semiconductor material, and cannot form a polyacid/semiconductor heterojunction. There has been no report on the study of polyacids to form heterojunctions with semiconductor materials and to be used as gas sensing. Therefore, the deep research on the gas sensing performance of the polyacid/semiconductor heterojunction material has become a key scientific problem for developing the application of the polyacid in devices such as gas sensors and the like. In addition, the influence of the structure of polyacid on gas sensing performance has not been fully revealed and studied, which limits the development and application of polyacid/semiconductor materials in the field of devices such as gas sensors. Thus, we introduced the polyacid to SnO 2 @WO 3 Two heterojunctions are formed, thereby obviously improving WO 3 The detection performance of the gas sensor.
Disclosure of Invention
The invention aims to provide a semiconductor/polyacid/semiconductor series heterojunction material and a preparation method thereof for the first time. Wherein the material is SnO 2 @POMs@WO 3 The structure of the three-layer coaxial nanofiber is shown in figure 1, a core layer is tin oxide, a middle layer is polyacid, a shell layer is tungsten oxide, and the three substances are distributed in a three-layer cable shape. Phosphomolybdic acid (PMo) with a polyacid of the Keggin type 12 ) Phosphotungstic acid (PW) 12 ) And silicotungstic acid (SiW) 12 ) The preparation method can be prepared by a coaxial electrostatic spinning technology and a calcining oxidation mode.
The second purpose of the invention is to solve the scientific problem of high electron hole recombination rate of the semiconductor gas-sensitive material. The material prepared by the invention has two heterogeneous interfaces connected in series, and can promote the migration of current carriers and inhibit the electron hole recombination, thereby improving the gas-sensitive performance of the material. And SnO without addition of polyacid 2 @WO 3 Compared with fiber, SnO 2 @POMs@WO 3 The three-layer coaxial nanofiber has more excellent gas-sensitive performance.
It is a further object of the present invention to apply for the first time polyacids to WO-based 3 The gas sensor of (1) is used for investigating the promotion effect of polyacid on the gas-sensitive performance of organic gases such as ethanol, acetone and the like.
SnO provided by the invention 2 @POMs@WO 3 The three-layer coaxial nanofiber gas sensing material can be prepared by the following method:
firstly, dissolving a certain amount of ammonium metatungstate and PVP in an organic solvent, and stirring at room temperature to obtain a transparent and uniform shell precursor solution; then dissolving a certain amount of stannic chloride and PVP in an organic solvent, and stirring at room temperature to obtain a uniform and transparent core layer precursor solution; and dissolving a certain amount of polyacid and PVP in an organic solvent, and stirring at room temperature to obtain a transparent and uniform intermediate layer precursor solution. Then the solution is spun under a certain voltage by a coaxial electrostatic spinning technology to obtain SnO 2 @POMs@WO 3 Precursor fiber is calcined at high temperature to prepare SnO 2 @POMs@WO 3 Three layers of coaxial nanofibers (the morphology is shown in figure 2).
SnO prepared by the method 2 @POMs@WO 3 The three-layer coaxial nanofiber is characterized by X-ray powder diffraction (PXRD, shown in figure 3) to determine the composition. It can be found that the peak positions and peak intensities of the synthesized material and tin oxide pentaoxide are consistent in the XRD spectrum, which proves that the material synthesized by the above method is actually tin oxide and tungsten oxide, and the presence of polyacid in the XRD spectrum cannot be observed due to the small content of polyacid.
SnO provided by the invention 2 @POMs@WO 3 The application of the three-layer coaxial nanofiber gas sensing material in gas sensing has the following working conditions:
the above materials can be coated on the gas sensor shown in fig. 4. The gas sensor consists of Al with a pair of gold electrodes on the outer surface 2 O 3 Insulating ceramic tube, through Al 2 O 3 Ni-Gr alloy heating wire and four Pt wires in insulating ceramic tube and Al-coated Ni-Gr alloy heating wire 2 O 3 The sensor comprises a hexagonal base consisting of an outer surface of an insulating ceramic tube and a sensitive material film on a pair of gold electrodes, wherein four posts of the hexagonal base connected with four platinum wires are connected to four signal wires, the remaining two posts are connected with two heating wires, after a certain current is applied, the sensor exposed in the air has a stable resistance value, and when the sensitive material film is contacted with a certain amount of gas (ethanol) to be detected, the resistance value is reduced until the stable value is reached. According to the principle, when the sensor works under a certain current and a corresponding certain temperature, if the resistance value is reduced, the existence of the gas to be measured is indicated.
The tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material provided by the invention has the following characteristics:
1. the tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material has a SnO main body 2 @POMs@WO 3 The three-layer coaxial nanofiber comprises a core layer made of tin oxide, a middle layer made of polyacid, a shell layer made of tungsten oxide and three substances distributed in a three-layer cable shape.
2. The tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material is coated on a ceramic tube electrode and has a sensing effect on ethanol gas at a certain working temperature. The first application of the polyacid to the composition based on WO 3 The gas sensor of (1) is used for investigating the promotion effect of polyacid on the gas-sensitive performance of organic gases such as ethanol, acetone and the like. .
3. The tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material has the advantages of optimal response performance to 100ppm ethanol, high sensitivity, quick response and recovery rate, good selectivity to ethanol gas and good long-term stability.
Drawings
Fig. 1 is a structural schematic diagram of a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material.
FIG. 2 is a transmission electron microscope image and a high-power transmission electron microscope image of a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material.
Fig. 3 is an X-ray powder diffraction pattern of a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material.
Fig. 4 is a schematic structural diagram of the tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensor.
FIG. 5 is a curve diagram of response amplitude of a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material to 100ppm ethanol at different temperatures.
FIG. 6 is a graph of the dynamic response and recovery characteristics of a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material at 280 ℃ for 5ppm to 100ppm ethanol gas.
FIG. 7 is a graph of the dynamic response and recovery time of a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material to 100ppm ethanol gas at 280 ℃.
FIG. 8 is a bar graph of response characteristics of a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material to 100ppm of different types of gases at 280 ℃.
FIG. 9 is a graph of the response amplitude change of a tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material to 100ppm ethanol gas within 30 days.
Detailed Description
To further illustrate the present invention, the following examples are set forth without limiting the scope of the invention as defined by the appended claims.
This example is an SnO with the best content of the three groups of polyacids prepared in the summary of the invention 2 @POMs(PMo 12 、PW 12 、SiW 12 )@WO 3 Testing the performance of the gas sensor by adding SnO 2 @POMs(1％PMo 12 、3％PW 12 、3％SiW 12 )@WO 3 Gas sensor and SnO 2 @WO 3 The gas sensor is subjected to a comparative experiment to test the performance; here, the gas response amplitude of the gas sensor is defined as S ═ R a /R g Where Ra is the resistance in air and Rg is the resistance in the gas to be measured, and further, the response or recovery time is 90% of the time it takes for the resistance value of the gas sensor to stabilize after being added or removed from the gas bottle to be measured.
Specific example 1:
SnO is reacted as shown in FIG. 5 2 @POMs(1％PMo 12 、3％PW 12 、3％SiW 12 )@WO 3 Gas sensor and SnO 2 @WO 3 The gas sensor tests the response performance of 100ppm ethanol at different temperatures of 240-360 ℃; as can be seen from the figure, four groups of sensors all showed temperature-dependent sensing characteristics, SnO 2 @POMs(1％PMo 12 、3％PW 12 、3％SiW 12 )@WO 3 Gas sensor and SnO 2 @WO 3 The response of the gas sensor reaches the maximum value at 280 ℃; therefore, the following other gas sensitive performance tests were all performed at the optimum temperature of 280 ℃.
As shown in FIG. 6, SnO 2 @POMs(1％PMo 12 、3％PW 12 、3％SiW 12 )@WO 3 Gas sensor and SnO 2 @WO 3 The gas sensor is used for testing the dynamic response and recovery characteristics of ethanol gas with different concentrations of 5ppm to 100ppm at 280 ℃: the results show that the ethanol concentration increasesIn addition, the response value thereof gradually increases, and SnO 2 @3％PW 12 @WO 3 The gas sensor has the best sensitivity to ethanol, and the response can reach 8.8 at 100 ppm.
As shown in FIG. 7, by reacting SnO 2 @POMs(1％PMo 12 、3％PW 12 、3％SiW 12 )@WO 3 Gas sensor and SnO 2 @WO 3 The gas sensor carries out response recovery characteristic test on 100ppm ethanol at 280 ℃, and the result shows that SnO 2 @1％PMo 12 @WO 3 The response time and recovery time of the gas sensor are 1.8s and 69.1s respectively, and the response recovery time is fastest, which indicates that SnO 2 @1％PMo 12 @WO 3 The gas sensor has a rapid response and recovery rate to ethanol gas.
As shown in FIG. 8, by reacting SnO 2 @POMs(1％PMo 12 、3％PW 12 、3％SiW 12 )@WO 3 Gas sensor and SnO 2 @WO 3 The gas sensor is used for testing the response characteristics of 100ppm different types of gases at 280 ℃, wherein SnO 2 @3％PW 12 @WO 3 The gas response amplitude of the gas sensor to 100ppm ethanol gas reaches 9, which shows that SnO 2 @3％PW 12 @WO 3 The gas sensor has good selectivity to ethanol gas.
As shown in FIG. 9, by reacting SnO 2 @POMs(1％PMo 12 、3％PW 12 、3％SiW 12 )@WO 3 The gas sensor is subjected to a stability test for 30 days, and the result shows that SnO 2 @3％SiW 12 @WO 3 The response amplitude to the ethanol gas is always kept at about 5.5, which shows that SnO 2 @3％SiW 12 @WO 3 The gas sensor has good long-term stability to ethanol.
Claims (4)
1. A tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material is characterized in that: has gas sensing performance, is a tin oxide/polyacid/tungsten oxide composite material with a molecular formula of SnO 2 @POMs@WO 3 The polyacid is Keggin typePhosphomolybdic acid, phosphotungstic acid or silicotungstic acid.
2. The tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material of claim 1, characterized in that: the gas sensor is prepared by a coaxial electrostatic spinning technology and a calcining oxidation mode, and is manufactured by coating a sensitive material film.
3. The tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material according to claim 1, characterized in that: under a certain working temperature, the existence of ethanol gas in the air can be detected by utilizing the change of an electrochemical signal, so that gas sensing is realized.
4. The tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material according to claim 1, characterized in that: the main body is three layers of coaxial nanofiber materials, a core layer is tin oxide, a middle layer is polyacid, a shell layer is tungsten oxide, the three materials are distributed in a three-layer cable shape, and the composition and the structure of the materials are determined; the material can stably exist on the electrode of the ceramic tube in the form of a film, so that the gas-sensitive reaction can be directly carried out in the air; the gas-sensitive reaction method is simple, the recovery is complete, and the environment is not polluted; the gas-sensitive film can be repeatedly used, and the gas sensitivity can still be maintained.
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| CN101874274A (en) * | 2007-11-27 | 2010-10-27 | 玛丽亚·斯特罗姆 | Composite materials including an intrinsically conducting polymer, and methods and devices |
| CN102331443A (en) * | 2011-07-13 | 2012-01-25 | 东华大学 | Acetone gas sensor and manufacturing method thereof |
| CN105606660A (en) * | 2015-12-24 | 2016-05-25 | 东北师范大学 | Gas-sensitive material for detecting NO2 and method for manufacturing gas-sensitive element made of gas-sensitive material |
| CN105628748A (en) * | 2015-12-24 | 2016-06-01 | 东北师范大学 | Platinum-loaded tin dioxide nanofiber gas-sensitive material and gas-sensitive element made from same |
| CN108760629A (en) * | 2018-05-22 | 2018-11-06 | 青海大学 | A kind of preparation method and applications of multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array |
| CN112578007A (en) * | 2020-12-02 | 2021-03-30 | 长春理工大学 | Indium oxide-polyacid composite gas sensing material and preparation method thereof |
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