CN109682867B - Micron-sized tin dioxide gas-sensitive material and preparation method and application thereof - Google Patents
Micron-sized tin dioxide gas-sensitive material and preparation method and application thereof Download PDFInfo
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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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Abstract
The invention discloses a micron-sized dioxygenPreparing tin dichloride and ethanol into a solution; and then transferring the mixture into a reaction kettle, reacting for a certain time, cooling a reaction system to obtain a mixed solution containing solid tin dioxide, and centrifuging and drying to obtain the faint yellow pure-phase tin dioxide micron particles. The invention is micron SnO2Provides a brand new solution idea and process flow in the aspect of green and environment-friendly industrial production, and has simple and easy method and process and good repeatability. And the whole reaction system has no pollution to the environment, and is a green and environment-friendly micron powder synthesis process. The gas sensor has strong practicability and better application prospect and economic benefit.
Description
Technical Field
The invention belongs to the technical field of synthesis of nano gas-sensitive materials and sensors, and particularly relates to a micron-sized tin dioxide gas-sensitive material as well as a preparation method and application thereof.
Background
With the progress of science and technology, the living standard of people is gradually improved, but the gas emitted by the industry, the agriculture and the daily activities of people is increased. Some of these gases are flammable and explosive, such as hydrogen, alcohol, methane, etc.; some are toxic, such as formaldehyde, hydrogen sulfide, carbon monoxide, and the like; the detection of these gases is a difficult problem to be solved, which has great significance for production and life, and the gas sensor plays an indispensable role.
The gas sensor can detect the components and the concentration of the gas and convert related information into a usable output signal, thereby having the functions of gas detection, alarm and the like. Gas sensors can be classified so far into the following categories: the gas sensor is a gas sensor which is most widely used due to the advantages of high sensitivity, low cost, stable performance and the like. Whereas in these semiconductor gas sensors, SnO2And is the gas sensitive material which is researched and applied most.
Tin dioxide is an important wide band gap (3.6-4.0eV) metal oxide halfThe crystal of the conductor material is rutile structure, and the unit cell is body-centered orthorhombic parallelepiped. Tin dioxide is useful as a gas sensitive material mainly because its resistance changes when it contacts a gas at a certain temperature, and in addition, because tin dioxide is an N-type semiconductor, its resistance decreases when it adsorbs a reducing gas and increases when it adsorbs an oxidizing gas. In terms of preparation process, the current methods for preparing tin dioxide are generally classified into solution methods, solid precursor thermal conversion methods, electrochemical deposition methods, thermal oxidation methods and the like. Tin dioxide (SnO) with different morphologies prepared by different methods2) The gas-sensitive materials have very different gas-sensitive properties. For example, a series of tin dioxide (SnO) with different diameters are prepared by taking carbon spheres as templates2) Hollow microspheres, hollow microspheres having a crystal size of 12.7nm were found to be resistant to nitrogen dioxide (NO)2) The most sensitive. E.g. Chiu et al, using SnCl4The nano particles with the size of 3.0nm prepared by a hydrothermal method and the surface area of the nano particles reaches 130m2(ii) a response to 25mg/L (ppm) ethanol of 26 at 220 ℃ with response and recovery times of 30s and 18s, respectively. Although SnO with micro-nano structures with different morphologies and doped with different metals and metal oxides is prepared by the method2Gas sensor, the gas sensing performance of which is more traditional SnO2The gas sensor is greatly improved, but still has some problems, such as poor selectivity, low working temperature, slow response and recovery time, complex preparation process, and more selected raw materials which are harmful to the environment and human health, so how to improve the selectivity and sensitivity of the dioxide to the gas, reduce the working temperature and optimize the preparation process is still a research hotspot in the future.
In conclusion, the research on the preparation process of the high-sensitivity micron-sized tin dioxide gas-sensitive material not only has important academic value, but also has important practical value, and therefore, the synthesis process for preparing and researching the high-sensitivity micron-sized tin dioxide gas-sensitive material is very important.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a simple, green and high-purity micron-sized tin dioxide gas-sensitive material, a preparation method and application thereof aiming at the defects in the prior art, the whole process is simple, pollution-free, simple in operation process and high in repeatability, high-purity tin dioxide powder can be obtained, and a sensor manufactured by the material has the advantages of high sensitivity, quick response and recovery time and the like under low concentration to ethanol gas.
The invention adopts the following technical scheme:
a preparation method of a micron-sized tin dioxide gas-sensitive material comprises the steps of preparing tin dichloride and ethanol into a solution; and then transferring the mixture into a reaction kettle, reacting for a certain time, cooling a reaction system to obtain a mixed solution containing solid tin dioxide, and centrifuging and drying to obtain the faint yellow pure-phase tin dioxide micron particles.
Specifically, 1-2 mmol of tin dichloride is added into ethanol, and the ethanol accounts for 70-80% of the volume of the reaction kettle.
Specifically, the prepared solution is transferred into a reaction kettle, the temperature is raised to 160-240 ℃ at the speed of 5-10 ℃/min, and the mixed solution containing solid tin dioxide is obtained after heat preservation treatment.
Further, the time of heat preservation treatment is 4-8 h.
Further, the set temperature of the reaction kettle is 180-220 ℃.
Specifically, the speed of centrifugal treatment is 5000-10000 r/min, and the time is 3-6 min.
Furthermore, the number of times of centrifugation is 2-4.
Specifically, the drying treatment temperature is 60-80 ℃, and the drying treatment time is 2-6 h.
The other technical scheme is that the micron-sized tin dioxide microparticles have the particle size of 1-3 microns.
The invention also provides a gas sensor prepared from the micron-sized tin dioxide micron particles.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the preparation method of the micron-sized tin dioxide gas-sensitive material, raw materials and generated solution in the whole process are easy to process and pollution-free, the preparation cost is low, the operation process is simple, the repeatability is high, the high-purity micron-sized spherical tin dioxide powder can be prepared, the whole reaction system has no pollution to the environment, and the preparation method is a green and environment-friendly micron powder synthesis process. The gas sensor has strong practicability and better application prospect and economic benefit.
The invention also discloses a gas sensor, the gas sensor prepared from the tin dioxide powder prepared by the method has excellent gas-sensitive performance, the response to alcohol is about 10 times of that of the tin dioxide gas sensor sold in the market, and in addition, the gas sensor still has the advantages of high sensitivity to alcohol gas under low concentration (1ppm), quick response recovery time, low working temperature and the like, and in addition, the gas sensor also has higher response to formaldehyde gas.
In conclusion, the invention is micron SnO2Provides a brand new solution idea and process flow in the aspect of green and environment-friendly industrial production. The method has simple and easy process and good repeatability. And the whole reaction system has no pollution to the environment, and is a green and environment-friendly micron powder synthesis process. The gas sensor has strong practicability and better application prospect and economic benefit.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is an XRD spectrum of example 1;
FIG. 2 is an SEM photograph of example 1;
FIG. 3 is an XRD spectrum of example 2;
FIG. 4 is an SEM photograph of example 2;
FIG. 5 is the XRD pattern for example 3;
FIG. 6 is an SEM photograph of example 3;
FIG. 7 is a graph showing the response of a gas sensor made of tin dioxide powder prepared by the method of the present invention in 100ppm ethanol gas at different operating temperatures;
FIG. 8 shows the response of a gas sensor made of tin dioxide powder prepared by the method of the present invention to ethanol gases of different concentrations;
FIG. 9 shows the response time and recovery time of a gas sensor made of tin dioxide powder prepared by the method of the present invention in 100ppm ethanol gas concentration;
FIG. 10 is a cycle test of a gas sensor made of tin dioxide powder prepared by the method of the present invention at a concentration of 100ppm ethanol gas;
FIG. 11 is a graph showing the response of a gas sensor made of tin dioxide powder prepared by the method of the present invention to four gases (ammonia, xylene, acetone, ethanol) at a concentration of 100 ppm;
FIG. 12 is a graph showing the comparison between the response of a gas sensor made of tin dioxide powder prepared by the method of the present invention and that of a commercially available tin dioxide sensor.
Detailed Description
The invention provides a preparation method of a micron-sized tin dioxide gas-sensitive material, which adopts conventional tin dichloride to prepare a solution; then transferring the mixture into a reaction kettle, reacting for a certain time, cooling a reaction system, centrifuging and drying to obtain pure-phase tin dioxide SnO2The micron particles overcome the defects that the prior art route adopts sodium hydroxide strong base as a precursor, thereby causing ecological pollution and causing danger to human bodies.
The invention relates to a preparation method of a micron-sized tin dioxide gas-sensitive material, which comprises the following steps:
s1, placing 1-2 mmol of tin dichloride into a certain amount of ethanol solvent, wherein the amount of the ethanol solvent is 70-80% of the capacity of the reaction kettle, and preparing into a solution;
s2, transferring the solution prepared in the step S1 into a reaction kettle, heating to 160-240 ℃ at a heating rate of 5-10 ℃/min, then preserving heat for 4-8 hours, reacting the solution in the process, and obtaining a mixed solution containing solid tin dioxide after the reaction is finished;
preferably, the set temperature of the reaction kettle is 180-220 ℃.
S3, taking the mixed solution containing the solid tin dioxide out of the reaction kettle, transferring the mixed solution into a centrifugal tube for centrifugal separation, wherein the centrifugal rate is 5000-10000 r/min, the time is 3-6 min, and the times are 2-4 times, so that the solid tin dioxide is obtained;
and S4, transferring the solid tin dioxide to a drying device for drying at the drying temperature of 60-80 ℃, and drying for 2-6 hours to obtain the finished product tin dioxide powder.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Weighing 1mmol of tin dichloride, dissolving the tin dichloride in 30mL of absolute ethyl alcohol, and stirring until the tin dichloride is dissolved to obtain a clear and transparent solution;
then transferring the transparent solution into a reaction kettle, then putting the reaction kettle into an oven for heating, heating the reaction kettle to 220 ℃, and then preserving heat for 6 hours, wherein the heating process of heating the reaction kettle is started from room temperature and is heated to 160 ℃ at the heating rate of 5 ℃/min;
in the process, tin dichloride in the transparent solution is subjected to chemical reaction in absolute ethyl alcohol to generate a mixed solution containing solid tin dioxide;
after the heat preservation time is reached, naturally cooling the reaction kettle to room temperature, taking the mixed solution out of the reaction kettle, and placing the mixed solution in a centrifugal machine for centrifugal separation, wherein the centrifugal rate of the centrifugal machine is set to 8000r/min, the centrifugal time is 3min, and the centrifugal times are 3 times;
after the centrifugal separation by the centrifuge, the solid tin dioxide is collected, and the solid tin dioxide is dried in a drying device, for example, at 60 ℃ for 6 hours, and after the drying, light yellow tin dioxide powder is obtained.
Example 2
Weighing 1mmol of tin dichloride, dissolving the tin dichloride in 35mL of absolute ethyl alcohol, and stirring until the tin dichloride is dissolved to obtain a clear and transparent solution;
then transferring the transparent solution into a reaction kettle, then putting the reaction kettle into an oven for heating, heating the reaction kettle to 200 ℃, and then preserving heat for 6 hours, wherein the heating process of heating the reaction kettle is started from room temperature and is heated to 240 ℃ at the heating rate of 10 ℃/min;
in the process, tin dichloride in the transparent solution is subjected to chemical reaction in absolute ethyl alcohol to generate a mixed solution containing solid tin dioxide;
after the heat preservation time is reached, naturally cooling the reaction kettle to room temperature, taking the mixed solution out of the reaction kettle, and placing the mixed solution in a centrifuge for centrifugal separation, wherein the centrifugal rate of the centrifuge is set to 5000r/min, the centrifugal time is 6min, and the centrifugation times are 4 times;
after the centrifugal separation by the centrifuge, the solid tin dioxide is collected, and the solid tin dioxide is dried in a drying device, for example, at 80 ℃ for 2 hours, and after the drying, light yellow tin dioxide powder is obtained.
Example 3:
weighing 1mmol of tin dichloride, dissolving the tin dichloride in 40mL of absolute ethyl alcohol, and stirring until the tin dichloride is dissolved to obtain a clear and transparent solution;
then transferring the transparent solution into a reaction kettle, then putting the reaction kettle into an oven for heating, heating the reaction kettle to 180 ℃, and then preserving heat for 4 hours, wherein the heating process of heating the reaction kettle is started from room temperature and is heated to 180 ℃ at the heating rate of 8 ℃/min;
in the process, tin dichloride in the transparent solution is subjected to chemical reaction in absolute ethyl alcohol to generate a mixed solution containing solid tin dioxide;
after the heat preservation time is reached, naturally cooling the reaction kettle to room temperature, taking the mixed solution out of the reaction kettle, and placing the mixed solution in a centrifugal machine for centrifugal separation, wherein the centrifugal rate of the centrifugal machine is set to 10000r/min, the centrifugal time is 5min, and the centrifugal times are 2 times;
after the centrifugal separation by the centrifuge, the solid tin dioxide is collected, and the solid tin dioxide is dried in a drying device, for example, at 70 ℃ for 4 hours, to obtain pale yellow tin dioxide powder.
Example 4
Weighing 2mmol of tin dichloride, dissolving the tin dichloride in 40mL of absolute ethyl alcohol, and stirring until the tin dichloride is dissolved to obtain a clear and transparent solution;
then transferring the transparent solution into a reaction kettle, then putting the reaction kettle into an oven for heating, heating the reaction kettle to 200 ℃, and then preserving heat for 8 hours, wherein the heating process of heating the reaction kettle is started from room temperature and is heated to 200 ℃ at the heating rate of 5 ℃/min;
in the process, tin dichloride in the transparent solution is subjected to chemical reaction in absolute ethyl alcohol to generate a mixed solution containing solid tin dioxide;
after the heat preservation time is reached, naturally cooling the reaction kettle to room temperature, taking the mixed solution out of the reaction kettle, and placing the mixed solution in a centrifugal machine for centrifugal separation, wherein the centrifugal rate of the centrifugal machine is set to 7000r/min, the centrifugal time is 5min, and the centrifugation times are 4 times;
after the centrifugal separation by the centrifuge, the solid tin dioxide is collected, and the solid tin dioxide is dried in a drying device, for example, at 70 ℃ for 5 hours, and after the drying, light yellow tin dioxide powder is obtained.
In addition, in the method of the invention, a reaction kettle made of a lining material can be selected, and other heating rates can be adopted for controlling the heating of the reaction kettle as long as the lining of the reaction kettle does not chemically react with tin dichloride.
Referring to FIGS. 1, 3 and 5, the tin dioxide obtained by the method of the present invention is scanned at 20 to 80 degrees using an X-ray diffractometer, and all diffraction peaks and SnO2The standard card (PDF # 04-009-.
Referring to fig. 2, 4 and 6, it can be seen from the SEM morphology photographs that the tin dioxide prepared by the method of the present invention is spherical, and the distribution of the tin dioxide is uniform, and the diameter of the microsphere is about 1 to 3 micrometers.
Referring to fig. 7, in the ethanol gas with a fixed concentration of 100ppm, the gas sensor prepared from the tin dioxide powder prepared by the method of the present invention can exhibit a high response value of 24.9 and a fastest response time of 3 seconds at a low operating temperature (230 ℃). Compared with other reported tin dioxide gas sensors, the sensor prepared by the method has lower working temperature.
Referring to fig. 8, the gas sensor made of the tin dioxide powder prepared by the method of the present invention has a response to ethanol gas with different concentrations, especially in a low ethanol concentration environment (1ppm), still has a high response (7.24), and has a fast response and recovery time.
Referring to fig. 9, the response time and recovery time of the gas sensor made of the tin dioxide powder prepared by the method of the present invention in the concentration of 100ppm ethanol gas reached 3s and 24 s.
Referring to fig. 10, in a cycle test of a gas sensor made of the tin dioxide powder prepared by the method of the present invention in an ethanol gas concentration of 100ppm, response values of the sensor in six cycle tests are substantially unchanged, which indicates that the sensor has stability.
Referring to fig. 11, the response of the gas sensor made of the tin dioxide powder prepared by the method of the present invention to four gases (ammonia, xylene, acetone, ethanol) with 100ppm concentration at the optimal working temperature (230 ℃) is found to be the highest response value to ethanol, so that the sensor has high selectivity to ethanol gas.
Referring to fig. 12, the response of the gas sensor made of the tin dioxide powder prepared by the method of the present invention to ethanol gas at different temperatures is compared with that of the commercially available tin dioxide gas sensor, such as the westxing microelectronic MQ-3 gas sensor, and as shown in fig. 12, the response of the gas sensor made of the tin dioxide powder prepared by the method of the present invention to ethanol gas at the optimal operating temperature, such as 230 ℃, is about 10 times that of the commercially available tin dioxide gas sensor, such as the westxing microelectronic MQ-3 gas sensor, to ethanol gas.
The above contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention should not be limited thereby, and any modification made on the basis of the technical idea proposed by the present invention falls within the protection scope of the claims of the present invention.
Claims (3)
1. A preparation method of a micron-sized tin dioxide gas sensitive material is characterized in that 2mmol of tin dichloride is added into ethanol to prepare a solution, and the ethanol accounts for 80% of the capacity of a reaction kettle; and then transferring the mixture into a reaction kettle, wherein the set temperature of the reaction kettle is 220 ℃, the temperature is increased to 240 ℃ at the speed of 10 ℃/min, the mixture containing solid tin dioxide is obtained after heat preservation treatment is carried out for 8 hours, the mixture containing solid tin dioxide is obtained after a reaction system is cooled, light yellow pure-phase tin dioxide micron particles are obtained through centrifugation and drying, the centrifugation treatment frequency is 4 times, the centrifugation treatment speed is 10000r/min, the time is 6min, and the drying treatment temperature is 80 ℃ and the time is 6 hours.
2. The micron-sized tin dioxide microparticles prepared by the method of claim 1, wherein the particle size of the tin dioxide microparticles is 1-3 microns.
3. A gas sensor made using micron-sized tin dioxide microparticles made by the method of claim 1.
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| CN111229198A (en) * | 2020-03-02 | 2020-06-05 | 陕西科技大学 | Amorphous/crystalline structure SnO2Preparation method of @ GO heterojunction composite material and photocatalytic application thereof |
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