CN109502632B - Multistage SnO2Preparation method and application of nanotube-shaped gas-sensitive material - Google Patents
Multistage SnO2Preparation method and application of nanotube-shaped gas-sensitive material Download PDFInfo
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Abstract
The invention discloses a multistage SnO2The preparation method of the nanotube-shaped gas-sensitive material comprises the following steps: (1) adding PVP into ethylene glycol, stirring, and performing ultrasonic treatment to obtain a solution a; (2) adding molybdenum oxide nano-rods into the alpha solutionUniformly dispersing in the solution to obtain a solution b; (3) adding a stannous chloride solution and a thioacetamide solution into the solution b, stirring, transferring into a reaction kettle, and carrying out constant-temperature hydrothermal treatment for 10-14 h; (4) cooling, centrifuging and collecting with anhydrous ethanol, transferring the obtained precipitate to a beaker with anhydrous ethanol, adding ammonia water, stirring for 1-2h, centrifuging and collecting, and drying the obtained precipitate to obtain SnS2(ii) a (5) The obtained SnS2And putting the mixture into a tubular furnace for calcining to obtain the catalyst. The method has the advantages of cheap and easily obtained raw materials, simple operation method, low energy consumption, strong repeatability and high yield, is suitable for batch production, and can prepare the multistage SnO2The nano tubular gas sensitive material can be used for materials such as sensors, catalysts, catalyst carriers and the like, and has good application prospect.
Description
Technical Field
The invention relates to the technical field of gas-sensitive materials, in particular to a multistage SnO2A preparation method and application of a nano-tube gas-sensitive material.
Background
In recent years, development of nanotechnology has greatly promoted development and application of functional materials. The size, morphology and components of the nano material can greatly influence the properties of the nano material, so that the application prospect of the nano material is influenced. So far, the modulation of two-dimensional lamellar, hollow tubular or three-dimensional multilevel semiconductor nano-structures and multi-components has attracted great interest to researchers, and becomes a new hot spot for nano-material research. The material has the advantages of large specific surface area and open structure, so the material has extremely important application value in the field of gas sensitive materials.
The gas sensitive material relates to the interaction between the surface of the sensitive material and adsorbed gas molecules, and the electrochemical performance of the sensitive material is changed through charge transfer between the surface of the sensitive material and the adsorbed gas molecules to generate a gas sensitive signal. What is more critical in the above process is to improve the interaction effect between the sensitive material and the gas molecules. Therefore, the specific surface area of the gas-sensitive nano material is improved, and the sensitivity is also a key direction for the research of the gas-sensitive material nowadays.
Most of the traditional methods for preparing the nano gas-sensitive material need complicated steps, expensive instruments and harsh reaction conditions, and volatile and toxic reagents are used, so that the method has influence on human health and the surrounding environment. Therefore, the multi-stage nano superstructure gas-sensitive material with optimized structure and excellent performance obtained by selecting a simple, economic and environment-friendly synthesis method is also the development trend of the gas-sensitive material.
Disclosure of Invention
The invention aims to: aiming at the problems, the multistage SnO is provided2Preparation method and application of nanotube-shaped gas-sensitive material, and the method has the advantages of low preparation cost, environmental friendliness, strong repeatability and multilevel SnO2The nano material of the nanotube superstructure has a large specific surface area, and is widely applied to the fields of transparent conductive films, gas sensors, photocatalysis, solar energy conversion and the like.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
multistage SnO2The preparation method of the nanotube-shaped gas-sensitive material comprises the following steps:
(1) adding PVP into ethylene glycol, stirring, and then carrying out ultrasonic treatment until the solution is clear to obtain a solution a;
(2) adding molybdenum oxide nanorods into the solution a, and stirring until the molybdenum oxide is uniformly dispersed in the solution a to obtain a solution b;
(3) adding a stannous chloride solution and a thioacetamide solution into the solution b, stirring, transferring into a reaction kettle, and carrying out constant-temperature hydrothermal treatment for 10-14 h;
(4) cooling, centrifuging with anhydrous ethanol, collecting, repeating for 3-6 times, transferring the obtained precipitate to beaker with anhydrous ethanol, adding ammonia water, stirring for 1-2 hr, centrifuging with anhydrous ethanol, collecting, cleaning for 3-6 times, and drying the obtained precipitate to obtain SnS2；
(5) The obtained SnS2And (5) calcining in a tubular furnace in an air atmosphere to obtain the catalyst.
Preferably, the solid-to-liquid ratio of the PVP to the ethylene glycol is 1: 45-100.
Preferably, the addition amount of the molybdenum oxide is 0.05-0.15% of the weight of the solution a.
Preferably, the mass ratio of the stannous oxide solution to the thioacetamide solution is 1: 1-1.2; the total weight of the stannous chloride solution and the thioacetamide solution is 10-18% of the weight of the solution b.
Preferably, the stannous oxide solution is prepared by dissolving 0.5-0.9g of stannous chloride in 10mL of ethylene glycol; the thioacetamide solution is prepared by dissolving 0.1-0.5g thioacetamide in 10mL of ethylene glycol.
Preferably, in the step (3), the reaction kettle is a stainless steel reaction kettle with a 50mL polytetrafluoroethylene lining, and the temperature of the constant temperature hydrothermal process is 150-.
Preferably, in the step (4), the drying temperature is 40-50 ℃ and the drying time is 8-14 h.
Preferably, in step (5), the calcination temperature is 380-420 ℃, the calcination time is 20-26h, and the temperature rise rate is 5 ℃/min.
The invention also provides the multistage SnO prepared by the method2The application of the nanotube gas sensitive material in transparent conducting film, sensor, catalyst and catalyst carrier material.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
(1) multi-stage SnO of the present invention2Preparation method of nanotube-shaped gas-sensitive material, directly mixing SnS2Conversion of hollow tubes into multi-stage SnO2The nano tubular gas sensitive material adopts a simple hydrothermal method and an annealing treatment technology, has cheap and easily obtained raw materials and is environment-friendly; using molybdenum oxide as template and SnS2Gas-sensitive material prepared by in-situ conversion of hollow tube precursor and large amount of SnO2The nano-sheets are stacked to form a novel tubular structure, and a unit SnO is basically constructed2The thickness of the nano-sheet is about 4nm, the nano-sheets are stacked in a multi-stage three-dimensional structure, the specific surface area and the number of diffusion channels are obviously increased, and the improvement of the performance of the gas sensor is hopefully assisted.
(2) The raw materials of the invention are cheap and easy to obtain, and the adopted preparation method is environment-friendly, low in hydrothermal temperature and low in energy consumption.
(3) The prepared multistage SnO2The gas-sensitive material of the nanotube superstructure is SnS with an easily flaky structure2The hollow pipe is formed by in-situ conversion, the appearance is special and rare, and the contact specific surface area is large.
(4) Prepared multistage SnO2The gas sensitive material with the nanotube superstructure can be used for materials such as sensors, catalysts, catalyst carriers and the like, and has good application prospect.
Drawings
FIG. 1 is a SnS prepared in example 12Conversion of hollow tubes into multi-stage SnO2SEM image of gas sensitive material of nanotube superstructure;
FIG. 2 is SnS prepared in example 22Conversion of hollow tubes into multi-stage SnO2SEM image of gas sensitive material of nanotube superstructure;
FIG. 3 is SnS prepared in example 12Conversion of hollow tubes into multi-stage SnO2A TEM image of the gas sensitive material of the nanotube superstructure;
FIG. 4 is SnS prepared in example 22Conversion of hollow tubes into multi-stage SnO2A TEM image of the gas sensitive material of the nanotube superstructure;
FIG. 5 shows SnS prepared in example 12And SnO2The XRD pattern of (a) is the precursor SnS2The diffraction peak pattern of (a), SnO2Diffraction peaks.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to preferred embodiments. It should be noted, however, that the numerous details set forth in the description are merely for the purpose of providing the reader with a thorough understanding of one or more aspects of the present invention, which may be practiced without these specific details.
The ethylene glycol used in the invention has a volume content of 29.6% and a density (20 ℃) of 1.041.
Example 1
Multistage SnO2The preparation method of the nanotube-shaped gas-sensitive material comprises the following steps:
(1) adding 0.45g of PVP (MW.58000) into 25ml of ethylene glycol, stirring for 30min, and carrying out ultrasonic treatment for 10min until the solution is clear to obtain a solution a;
(2) adding 15mg of molybdenum oxide nanorods into the solution a, and stirring for 1h until the molybdenum oxide is uniformly dispersed in the solution a to obtain a solution b;
(3) adding 1.6ml of stannous chloride solution (0.758g of stannous chloride dissolved in 10ml of ethylene glycol) and 1.6ml of thioacetamide solution (0.3g of thioacetamide dissolved in 10ml of ethylene glycol) into the solution b, stirring for 20min, transferring into a 50ml of stainless steel reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal treatment at the constant temperature of 160 ℃ for 12 h;
(4) cooling, collecting, centrifuging with anhydrous ethanol, collecting, repeating for 5 times, transferring the obtained precipitate with 20ml anhydrous ethanol into a beaker, adding 3ml concentrated ammonia water for removing molybdenum oxide template, stirring for 90min, centrifuging with anhydrous ethanol, collecting, repeating for 5 times, and drying the obtained precipitate at 45 deg.C for 12 h;
(5) the obtained SnS2Putting the mixture into a tubular furnace, calcining the mixture for 24 hours at the temperature of 400 ℃ in the air atmosphere, and raising the temperature at the speed of 5 ℃/min.
Example 2
(1) Adding 0.5g PVP (MW.58000) into 25ml of ethylene glycol, stirring for 30min, and carrying out ultrasonic treatment for 10min until the solution is clear;
(2) adding 20mg of molybdenum oxide nano-rods into the solution a, and stirring for 1h until the molybdenum oxide is uniformly dispersed in the solution a;
(3) adding 1.6ml of stannous chloride solution (0.758g of stannous chloride dissolved in 10ml of ethylene glycol) and 1.6ml of thioacetamide solution (0.3g of thioacetamide dissolved in 10ml of ethylene glycol) into the solution b, stirring for 20min, transferring into a 50ml of stainless steel reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal treatment at constant temperature for 12 h;
(4) cooling, collecting, centrifuging with anhydrous ethanol, collecting, repeating for 5 times, transferring the obtained precipitate with 20ml anhydrous ethanol into a beaker, adding 3ml concentrated ammonia water, stirring for 90min, removing molybdenum oxide template, centrifuging with anhydrous ethanol, collecting, cleaning for 5 times, and drying the obtained precipitate at 45 deg.C for 10 h;
(5) the obtained SnS2Putting the mixture into a tubular furnace, calcining the mixture for 24 hours at the temperature of 400 ℃ in the air atmosphere, and raising the temperature at the speed of 5 ℃/min.
Example 3
Multistage SnO2The preparation method of the nanotube-shaped gas-sensitive material comprises the following steps:
(1) adding 0.45g of PVP (MW.58000) into 45ml of ethylene glycol, stirring for 30min, and carrying out ultrasonic treatment for 10min until the solution is clear to obtain a solution a;
(2) adding 24mg of molybdenum oxide nanorods into the solution a, and stirring for 1h until the molybdenum oxide is uniformly dispersed in the solution a to obtain a solution b;
(3) adding 2.18ml of stannous chloride solution (0.5g of stannous chloride dissolved in 10ml of ethylene glycol) and 2.62ml of thioacetamide solution (0.5g of thioacetamide dissolved in 10ml of ethylene glycol) into the solution b, stirring for 20min, transferring into a 50ml of stainless steel reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal treatment at the constant temperature of 150 ℃ for 14 h;
(4) cooling, collecting, centrifuging with anhydrous ethanol, collecting, repeating for 3 times, transferring the obtained precipitate with 20ml anhydrous ethanol into a beaker, adding 3ml concentrated ammonia water for removing molybdenum oxide template, stirring for 90min, centrifuging with anhydrous ethanol, collecting, repeatedly cleaning for 6 times, and drying the obtained precipitate at 40 deg.C for 14 h;
(5) the obtained SnS2Placing the mixture into a tubular furnace, calcining the mixture for 26 hours at 380 ℃ in the air atmosphere, and raising the temperature at the rate of 5 ℃/min.
Example 4
Multistage SnO2The preparation method of the nanotube-shaped gas-sensitive material comprises the following steps:
(1) adding 0.45g of PVP (MW.58000) into 20ml of ethylene glycol, stirring for 30min, and carrying out ultrasonic treatment for 10min until the solution is clear to obtain a solution a;
(2) adding 31.5mg of molybdenum oxide nanorods into the solution a, and stirring for 1h until the molybdenum oxide is uniformly dispersed in the solution a to obtain a solution b;
(3) adding 1.89ml of stannous chloride solution (0.9g of stannous chloride dissolved in 10ml of ethylene glycol) and 1.89ml of thioacetamide solution (0.1g of thioacetamide dissolved in 10ml of ethylene glycol) into the solution b, stirring for 20min, transferring into a 50ml of stainless steel reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal treatment at the constant temperature of 170 ℃ for 8 h;
(4) cooling, collecting, centrifuging with anhydrous ethanol, collecting, repeating for 3 times, transferring the obtained precipitate with 20ml anhydrous ethanol into a beaker, adding 3ml concentrated ammonia water for removing molybdenum oxide template, stirring for 90min, centrifuging with anhydrous ethanol, collecting, repeatedly cleaning for 6 times, and drying the obtained precipitate at 50 deg.C for 8 h;
(5) the obtained SnS2Placing the mixture into a tubular furnace, calcining the mixture for 20 hours at the temperature of 420 ℃ in the air atmosphere, and raising the temperature at the speed of 5 ℃/min.
The multistage SnO prepared in example 1 and example 22The gas-sensitive material with nanotube superstructure can be used for carrying out field emission electron scanning microscope (FE-SEM) experiment to obtain hollow tubular SnO shown in electron microscope photos of fig. 1 and fig. 22Countless nano-sheets are grown on the surface, and the nano-sheets are uniformly distributed in SnO like a flower shape2The surface greatly increases the specific surface area of the nanotube and improves the sensitivity of the material. FIGS. 3 and 4 show the multi-stage SnO prepared in examples 1 and 22Gas sensitive materials of nanotube superstructures, as can be observed in the figure, SnO2The thickness of the nano-sheets is about 4nm, and the nano-sheets are stacked in different directions to form a hollow tubular structure. As is clear from the diffraction peak of XRD pattern (a) in FIG. 5, SnS2Most diffraction peaks of the hollow tube precursor are all in contact with SnS2Corresponding to the phase (JCPDS No.23-0677), but having a distinct Sn layer on the (020) plane corresponding to 12.605 degrees of 2 theta2S3Diffraction peaks of the phase (JCPDS No.14-0619) indicating the presence of a trace amount of Sn in the precursor2S3(ii) a While the diagram (b) is pure tetragonal SnO2(JCPDS No.41-1445) showing a larger diffraction intensity than that of the diffraction peak shown in the graph (a), indicating that SnO was annealed2The crystallinity is higher, the grain size is larger, and the precursor is completely converted into SnO2No impurities are produced.
SnO2An n-type wide band gap semiconductor (Eg. 3.62eV) characterized by a small particle diameter, a large specific surface area, a small size effect,The surface and interface effects, the macroscopic quantum tunneling effect and the like are obvious, so that the method can be widely applied to scientific research and industrial application of gas sensors, resistors, transparent heating elements, catalysts, solar cells and the like.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (7)
1. A preparation method of a multistage SnO2 nanotube-shaped gas-sensitive material is characterized by comprising the following steps: the method comprises the following steps:
(1) adding PVP into ethylene glycol, stirring, and then carrying out ultrasonic treatment until the solution is clear to obtain a solution a;
(2) adding molybdenum oxide nanorods into the solution a, and stirring until the molybdenum oxide is uniformly dispersed in the solution a to obtain a solution b;
(3) adding a stannous chloride solution and a thioacetamide solution into the solution b, stirring, transferring into a reaction kettle, and carrying out constant-temperature hydrothermal treatment for 10-14 h;
(4) cooling, centrifugally collecting the precipitate by using absolute ethyl alcohol, repeating the steps for 3-6 times, transferring the obtained precipitate to a beaker by using absolute ethyl alcohol, adding ammonia water, stirring for 1-2 hours, centrifugally collecting the precipitate by using absolute ethyl alcohol, repeatedly cleaning for 3-6 times, and drying the obtained precipitate to obtain SnS 2;
(5) calcining the obtained SnS 2 in a tubular furnace in the air atmosphere to obtain the catalyst;
the mass ratio of the stannous oxide solution to the thioacetamide solution is 1: 1-1.2; the total weight of the stannous chloride solution and the thioacetamide solution is 10-18% of the weight of the solution b;
the multistage SnO2 nanotube-shaped gas-sensitive material is constructed by SnO2 nanosheets with the thickness of about 4nm, the sheets are stacked in a multistage three-dimensional structure, and a large number of sheets are stacked in different directions to form a hollow tubular structure.
2. The preparation method of the multistage SnO2 nanotube-shaped gas-sensitive material according to claim 1, characterized in that: the solid-liquid ratio of the PVP to the ethylene glycol is 1: 45-100.
3. The preparation method of the multistage SnO2 nanotube-shaped gas-sensitive material according to claim 1, characterized in that: the addition amount of the molybdenum oxide is 0.05-0.15% of the weight of the solution a.
4. The preparation method of the multistage SnO2 nanotube-shaped gas-sensitive material according to claim 1, characterized in that: the stannous oxide solution is prepared by dissolving 0.5-0.9g of stannous chloride in 10mL of ethylene glycol; the thioacetamide solution is prepared by dissolving 0.1-0.5g thioacetamide in 10mL of ethylene glycol.
5. The preparation method of the multistage SnO2 nanotube-shaped gas-sensitive material according to claim 1, characterized in that: in the step (3), the reaction kettle is a stainless steel reaction kettle with a 50mL polytetrafluoroethylene lining, and the temperature of the constant temperature hydrothermal process is 150-.
6. The preparation method of the multistage SnO2 nanotube-shaped gas-sensitive material according to claim 1, characterized in that: in the step (4), the drying temperature is 40-50 ℃ and the drying time is 8-14 h.
7. The preparation method of the multistage SnO2 nanotube-shaped gas-sensitive material according to claim 1, characterized in that: in the step (5), the calcining temperature is 380-420 ℃, the calcining time is 20-26h, and the heating rate is 5 ℃/min.
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