CN108910941B - Butterfly-shaped SnO2Two-dimensional nano material and preparation method and application thereof - Google Patents
Butterfly-shaped SnO2Two-dimensional nano material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a butterfly-shaped SnO2Two-dimensional nano material and its preparation method and application. Said butterfly shaped SnO2The two-dimensional nano material is SnSO4And SDBS as raw material, and is prepared by a two-step combined method of hydrothermal reaction and high-temperature oxidation annealing, wherein the butterfly-shaped SnO2The two-dimensional nano material has a two-dimensional butterfly shape and a rich surface defect structure, and has the characteristics of gas adsorption, surface activity, oxidation reduction and gas sensitivity. The preparation method comprises the steps of precursor solution preparation, main reaction, precursor separation and high-temperature oxidation heat treatment of the nano material. SnO applied in the shape of butterfly2The application of two-dimensional nano material in preparing gas sensor. Aiming at the existing preparation of two-dimensional SnO2The preparation process of the nano material is complicated, the cost is high, the large-scale preparation cannot be carried out, strong acid and strong base are added, and toxic and harmful organic solvents which are not good for the environment are added.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to butterfly-shaped SnO2Two-dimensional nano material and its preparation method and application.
Background
Since 2004, the preparation and application of various two-dimensional inorganic nanomaterials has entered a period of rapid development after Novoselov K S and Geim a K successfully used tape to exfoliate graphene flakes from highly oriented pyrolytic graphite. Due to the reduction of material dimension and the reduction of structural characteristic dimension, the two-dimensional nano materials such as nano sheets, nano films and the like have obvious surface effect, interface effect, small-size effect and macroscopic quantum tunnelThe channel effect, the dielectric confinement effect and the like make the material have novel and unique physical, electronic, chemical and optical characteristics different from the traditional material, so the material has wide application prospect in the aspects of photoelectric devices, sensors, microwave absorption, energy storage, catalysis and the like. SnO2As an important n-type semiconductor oxide functional material with a wide band gap (Eg =3.6eV, 300K), the material is widely used in the fields of gas sensing, photocatalysis, lithium ion batteries, capacitors, thin film resistors, solar cells, and the like. SnO2The two-dimensional nanostructures such as the nano-sheets, the nano-films and the like have large active specific surface area, better surface adsorption property and high surface activity, so the two-dimensional nanostructures have outstanding sensitive functional property to the change of external environments such as gas, light, electricity and the like, and have unique advantages in the aspects of designing novel nano-sensors, photocatalytic purification devices, liquid crystal displays, sensitized solar cells and the like. Preparation of two-dimensional SnO with controllable composition, dimension and morphology2Nanostructures are key to the design and construction of nanodevices and devices.
SnO obtained by different preparation methods2Two-dimensional nanomaterials have different structural characteristics such as different physical, chemical, morphological and surface properties. At present, two-dimensional-structure SnO with different micro-morphologies such as nano-sheets, nano-films and the like is synthesized at home and abroad by various preparation technologies2Nano materials such as physical sputtering deposition method, Chemical Vapor Deposition (CVD), template method, anodic oxidation method, chemical deposition method, sol-gel method, atomic layer deposition method, micro arc oxidation technique, solution combustion method, etc. Two-dimensional SnO preparation by adopting methods2When nano materials such as nano sheets, nano films and the like are adopted, expensive experimental instruments and equipment are often needed, most of the nano materials need severe experimental conditions and complicated experimental procedures, the reaction temperature is high, large-scale preparation cannot be carried out, and the actual requirements cannot be met. Also, some methods have difficulty controlling SnO2The composition, crystal form and morphology of the material. The hydrothermal method is a typical thermochemical method, and is favorable for controlling nucleation, growth, self-assembly and the like of crystals to form a nano structure with special morphology in a closed system under higher pressure and temperatureHas the characteristics of simple operation, low cost, green, easy scale production and the like, and is a method for preparing SnO2The important technology of nano material. In recent years, hydrothermal method has been used to synthesize some SnO with two-dimensional nanostructures of specific morphology2And (3) nano materials. In the hydrothermal synthesis, strong acid or strong base such as sodium hydroxide, potassium hydroxide, hydrochloric acid and the like are mostly basic conditions of the method, and toxic and harmful organic solvents which are not good for the environment are also mostly needed; more importantly, the two-dimensional SnO prepared by the hydrothermal method2The characteristics of the nano-sheets and nano-films, such as surface activity, surface adsorption, gas sensitivity, oxidation reduction and the like, are limited, and SnO is prevented2Application of two-dimensional nano material. Therefore, a simple, economic and green hydrothermal method is developed, the crystal morphology is regulated and controlled by utilizing the principles and modes of crystal nucleation, growth and self-assembly and adjusting the components and concentration of a reaction system and the properties of thermodynamics and the like of the reaction system, and a novel SnO with excellent surface activity is synthesized2The two-dimensional nano structure is necessary, which has important scientific significance for developing the synthesis of materials and the research of nano materials in new application fields.
Disclosure of Invention
The first purpose of the invention is to provide SnO with butterfly shape2A two-dimensional nanomaterial; the second purpose is to provide the SnO with butterfly shape2A preparation method of the two-dimensional nano material; the third purpose is to provide the SnO with butterfly shape2Application of two-dimensional nano material.
The first object of the present invention is achieved by said butterfly-shaped SnO2The two-dimensional nano material is SnSO4And SDBS as raw material, and is prepared by two steps of combining hydrothermal reaction and high-temperature oxidation annealing, wherein the SnO in the butterfly shape2The two-dimensional nano material has a two-dimensional butterfly shape and a rich surface defect structure, and has the characteristics of gas adsorption, surface activity, oxidation reduction and gas sensitivity.
The second purpose of the invention is realized by the steps of precursor solution preparation, main reaction, precursor separation and nano material preparation, which specifically comprises the following steps:
A. preparing a precursor solution:
1) accurately weighing Sodium Dodecyl Benzene Sulfonate (SDBS), stirring and dissolving the SDBS into deionized water at a stirring speed of 240-480 r/min to prepare an aqueous solution with a molar concentration of 0.04-0.20 mol/L to obtain a solution a;
2) SnSO precision weighing4Adding the solution into the solution a, and stirring the solution at a stirring speed of 480 to 720r/min for 60 to 180min to obtain a hydrothermal synthesis precursor reaction system b, wherein SnSO4The molar ratio of the SDBS to the SDBS is (1: 1) - (2: 1);
B. main reaction: heating the hydrothermal synthesis precursor reaction system b to 160-220 ℃ at a slow heating rate of 1-6 ℃/min, and carrying out heat preservation reaction at 160-220 ℃ for 12-60 h to obtain a reaction solution c; the slow heating rate is 1-6 ℃/min, and the main reason is to ensure that SnSO in a precursor reaction system is synthesized by hydrothermal synthesis4Slowly and fully hydrolyzing to fully form SnO crystal nucleus and crystal grain, and carrying out self-assembly under the induction of Sodium Dodecyl Benzene Sulfonate (SDBS) to finally form butterfly-shaped SnO precursor d.
C. Precursor separation: carrying out centrifugal separation on the reaction liquid c to obtain a hydrothermal reaction deposition product, namely a butterfly-shaped SnO precursor d; the size of each unit of butterfly-shaped SnO is 15-80 mu m, and the surface of each unit of butterfly-shaped SnO is smooth and has no obvious defect (see figure 2 specifically).
D. Preparing a nano material:
1) cleaning the butterfly-shaped SnO precursor d to remove reaction residues and reaction byproducts, and separating and drying to obtain a material e;
2) carrying out high-temperature oxidation annealing on the material e at the temperature of 550-800 ℃ to obtain the target object of butterfly-shaped SnO2Two-dimensional nanomaterials.
Butterfly shaped SnO from figure 32As can be seen from the FESEM appearance picture of the two-dimensional nano material, each unit is butterfly-shaped SnO2The size of the metal oxide is 15-80 μm, and is consistent with that of SnO. As can be seen from the TEM image pictures of FIGS. 2, 3, 4 and 5, butterfly-shaped SnO2The thickness of the lamella is 10-80 nm, and butterfly-shaped SnO is shown in figure 42High power of two-dimensional nano materialAs can be seen from the FESEM morphology picture, each unit is butterfly-shaped SnO2The surface of the wafer is grown with a plurality of protruding island-shaped surface defect structures, the size of the island-shaped protrusions is 50 nm-2 mu m, and the protruding island-shaped surface defect structures can increase SnO2The specific surface area of the material enhances the gas adsorption capacity of the material, and increases active sites for reaction with gas, thereby improving the gas sensitivity of the material.
The third object of the present invention is achieved by the butterfly-shaped SnO2The application of two-dimensional nano material in preparing gas sensor.
The invention aims at the existing synthesis method to prepare two-dimensional SnO2When nano materials such as nano sheets, nano films and the like need expensive experimental instruments and equipment, severe experimental conditions, complicated preparation procedures and higher cost, large-scale preparation cannot be carried out, strong acid, strong base and toxic and harmful organic solvents which are not good for the environment are added, the invention provides a simple, economic, green and easily-scaled hydrothermal synthesis method, only water is used as a solvent, strong acid, strong base and other toxic and harmful organic solvents are not added, and the concentration of Sodium Dodecyl Benzene Sulfonate (SDBS) in a hydrothermal reaction precursor solution and the concentration of the Sodium Dodecyl Benzene Sulfonate (SDBS) and a tin source SnSO are regulated by regulating the concentration of the Sodium Dodecyl Benzene Sulfonate (SDBS) in the hydrothermal reaction precursor solution4The two-dimensional butterfly-shaped SnO with novel and rich surface defects is prepared by utilizing the principles and modes of crystal nucleation, growth and self-assembly and regulating and controlling the crystal morphology by regulating the concentration of a reaction system and the properties of thermodynamics and the like of the reaction system2And (3) nano materials. The butterfly-shaped SnO2The surface adsorption and activity, the oxidation reduction, the gas sensitivity and other characteristics of the two-dimensional nano structure are greatly improved, and the two-dimensional nano structure has better sensitivity to acetaldehyde gas; and the gas sensitivity can be modulated by adjusting the heat treatment temperature, and the material can be used as a material for detecting acetaldehyde gas to manufacture an acetaldehyde gas sensitive device.
The invention has the advantages that:
(1) the invention prepares butterfly-shaped two-dimensional structure SnO by using hydrothermal method2In the process of the nano material, strong acid and strong base do not need to be added, only water is used as a solvent, and the precursor is prepared by changing the hydrothermal reactionThe self thermodynamics, kinetics and other properties of the system are controlled by the synthesis parameters of the solution, and butterfly-shaped SnO is realized2Self-assembly of a two-dimensional structure, simple, economic, green and easy to scale, and the obtained butterfly-shaped SnO2The two-dimensional structure has the characteristics of gas adsorption, surface activity, oxidation reduction, gas sensitivity and the like.
(2) SnO with butterfly-shaped two-dimensional structure2The nano material is used as an indirectly heated gas sensor made of a gas sensitive material, and has ultrahigh sensitivity, high selectivity, quick response and recovery characteristics and a detection limit of ppb level to acetaldehyde gas; and the sensitivity to acetaldehyde gas can be modulated by adjusting the heat treatment temperature. FIG. 6 is a butterfly-shaped two-dimensional structure SnO2The graph of the sensitivity reaction of the nano material as a gas sensitive material to various organic reducing gases can be obtained, and the butterfly-shaped two-dimensional structure SnO2The nanometer material as a gas sensitive material has ultrahigh sensitivity and excellent selectivity to acetaldehyde gas, and can be used for detecting the acetaldehyde gas.
(3) SnO according to butterfly-shaped two-dimensional structure2The gas sensitivity of the nano material is changed along with the heat treatment temperature, and the butterfly-shaped two-dimensional structure SnO can be realized by adjusting the heat treatment temperature2The modulation of the gas sensitivity performance of the nano material can customize materials with different acetaldehyde gas sensitivity performances to manufacture acetaldehyde gas sensitive devices.
Drawings
FIG. 1 is a butterfly-shaped two-dimensional structure SnO2Preparing technological process of nanometer material;
FIG. 2 is a FESEM morphology picture of a butterfly-shaped two-dimensional structure SnO precursor nano material;
FIG. 3 is a butterfly shaped SnO2FESEM appearance picture of two-dimensional nano material;
FIG. 4 is a butterfly shaped SnO2High power FESEM appearance picture of two-dimensional nanometer material;
FIG. 5 is a butterfly shaped SnO2TEM pictures of two-dimensional nanomaterials;
FIG. 6 shows butterfly SnO2The sensitivity performance graph of the two-dimensional nano material sensor to various gases;
FIG. 7 shows butterfly-shaped SnO prepared by the invention2FESEM appearance picture of two-dimensional nano material;
wherein (a), (b) and (c) are butterfly SnO prepared in examples 1, 2 and 3 respectively2A two-dimensional nanomaterial;
FIG. 8 is a butterfly-shaped SnO prepared in examples 1 to 32The relationship curve between the sensitivity of the sensor made of two-dimensional nano materials to 200ppm acetaldehyde and the heating voltage;
FIG. 9 is a butterfly-shaped SnO prepared in examples 1 to 32The sensitivity of the sensor made of the two-dimensional nano material is a curve of dynamic change along with the concentration of acetaldehyde when the heating voltage is 2.5V.
Detailed Description
The present invention is further illustrated by the following examples and the accompanying drawings, but the present invention is not limited thereto in any way, and any modifications or alterations based on the teaching of the present invention are within the scope of the present invention.
The butterfly-shaped SnO2The two-dimensional nano material is SnSO4And SDBS as raw materials are prepared by hydrothermal reaction, and the butterfly-shaped SnO2The two-dimensional nano material has a two-dimensional butterfly shape and a rich surface defect structure, and has the characteristics of gas adsorption, surface activity, oxidation reduction and gas sensitivity.
The butterfly-shaped SnO2The preparation method of the two-dimensional nano material comprises the steps of precursor solution preparation, main reaction, precursor separation and nano material preparation, and specifically comprises the following steps:
A. preparing a precursor solution:
1) accurately weighing Sodium Dodecyl Benzene Sulfonate (SDBS), stirring and dissolving the SDBS into deionized water at a stirring speed of 240-480 r/min to prepare an aqueous solution with a molar concentration of 0.04-0.20 mol/L to obtain a solution a;
2) SnSO precision weighing4Adding the mixture into the solution a and stirring the mixture at 480 to 720r/minStirring at a stirring rate of 60-180 min to obtain a hydrothermal synthesis precursor reaction system b, wherein SnSO4The molar ratio of the SDBS to the SDBS is (1: 1) - (2: 1);
B. main reaction: heating the hydrothermal synthesis precursor reaction system b to 160-220 ℃ at a slow heating rate of 1-6 ℃/min, and carrying out heat preservation reaction at 160-220 ℃ for 12-60 h to obtain a reaction solution c; the slow heating rate is 1-6 ℃/min, and the main reason is to ensure that SnSO in a precursor reaction system is synthesized by hydrothermal synthesis4Slowly and fully hydrolyzing to fully form SnO crystal nucleus and crystal grain, and carrying out self-assembly under the induction of Sodium Dodecyl Benzene Sulfonate (SDBS) to finally form butterfly-shaped SnO precursor d.
C. Precursor separation: carrying out centrifugal separation on the reaction liquid c to obtain a hydrothermal reaction deposition product, namely a butterfly-shaped SnO precursor d; the size of each unit of butterfly-shaped SnO is 15-80 mu m, and the surface of each unit of butterfly-shaped SnO is smooth and has no obvious defect (see figure 2 specifically).
D. Preparing a nano material:
1) cleaning the butterfly-shaped SnO precursor d to remove reaction residues and reaction byproducts, and separating and drying to obtain a material e;
2) carrying out high-temperature oxidation annealing on the material e at the temperature of 550-800 ℃ to obtain the target object of butterfly-shaped SnO2Two-dimensional nanomaterials.
Butterfly shaped SnO from figure 32As can be seen from the FESEM appearance picture of the two-dimensional nano material, each unit is butterfly-shaped SnO2The size of the metal oxide is 15-80 μm, and is consistent with that of SnO. As can be seen from the TEM image pictures of FIGS. 2, 3, 4 and 5, butterfly-shaped SnO2The thickness of the lamella is 10-80 nm, and butterfly-shaped SnO is shown in figure 42The high power FESEM appearance picture of the two-dimensional nano material can be seen, and each unit is butterfly-shaped SnO2The surface of the wafer is grown with a plurality of protruding island-shaped surface defect structures, the size of the island-shaped protrusions is 50 nm-2 mu m, and the protruding island-shaped surface defect structures can increase SnO2The specific surface area of the material enhances the gas adsorption capacity of the material, and increases active sites for reaction with gas, thereby improving the gas sensitivity of the material.
And B, a main reaction vessel is a reaction kettle with a polytetrafluoroethylene lining.
The temperature of the centrifugal separation in the step C is below 4 ℃.
And C, the rotation speed of centrifugal separation in the step C is 12000-15000 r/min.
And D) repeatedly cleaning by adopting acetone, deionized water and absolute ethyl alcohol during cleaning in the step 1).
D, the separation in the step 1) is carried out by filtering through a 100-mesh filter screen.
And D, drying in the step 1) is carried out for 12-24 hours at the temperature of 60-80 ℃.
And D) in the step 2), the high-temperature oxidation annealing is to heat the material e to 550-800 ℃ at the heating rate of 2-5 ℃/min, preserve the temperature for 60-120 min, and then cool the material e to the normal temperature at the cooling rate of 2-5 ℃/min.
The temperature rise rate of 2-5 ℃/min is to ensure that SnO is slowly and fully oxidized in an air atmosphere to generate phase change and generate SnO2And prevent the generation of strong stress in the SnO crystal due to too fast temperature rise and damage of the structure, so that the temperature is reduced at the temperature reduction rate of 2-5 ℃/min.
The butterfly-shaped SnO2The preparation method of the two-dimensional nano material comprises the following specific operations:
(1) preparing hydrothermal reaction precursor solution
a. Weighing a certain amount of Sodium Dodecyl Benzene Sulfonate (SDBS) (irreplaceability) by balance, completely dissolving the SDBS in deionized water with a certain volume, stirring for 60-90 minutes, and preparing into an aqueous solution with the molar concentration of 0.04-0.20 mol/L;
b. with SnSO4Weighing a certain amount of SnSO as a tin source (irreplaceability)4Adding the solution into the aqueous solution prepared in the step a, stirring for 60-180 minutes to prepare a hydrothermal synthesis precursor reaction system, and adding SnSO into the mixed aqueous solution4The molar ratio of the SDBS to the SDBS is 1: 1-2: 1;
(2) transferring the hydrothermal reaction precursor solution into a miniature reaction kettle with a polytetrafluoroethylene lining at 160-220 deg.CoThe temperature is kept at C temperature for 12 to 60 hoursThen naturally cooling to room temperature along with the furnace;
(3) carrying out centrifugal separation on the reacted solution to obtain a hydrothermal reaction deposition product, namely a butterfly-shaped SnO precursor;
(4) repeatedly cleaning the deposition product by using deionized water and absolute ethyl alcohol, removing reaction residues and reaction byproducts, and separating and drying the cleaned sample;
(5) the dried sample is placed at 550-800 DEGoHigh-temperature oxidation annealing is carried out under C to obtain butterfly-shaped SnO with rich defects2A two-dimensional nanomaterial;
(6) butterfly shaped SnO2The preparation process flow of the two-dimensional nano material is shown in figure 1, the butterfly-shaped SnO precursor prepared by hydrothermal reaction is shown in figure 2, and the butterfly-shaped SnO is obtained after high-temperature oxidation annealing2The two-dimensional nanomaterials are shown in fig. 3, 4 and 5, respectively.
The butterfly-shaped SnO2The application of the two-dimensional nano material is the butterfly-shaped SnO2The application of two-dimensional nano material in preparing gas sensor.
SnO with butterfly-shaped two-dimensional structure2The method of fabricating the gas sensor using the nanomaterial is not limited to the following method.
SnO with butterfly-shaped two-dimensional structure2The nanometer material is used as a gas sensitive material to manufacture an indirectly heated gas sensor. The manufacturing process of the gas sensor comprises the following steps:
a. formulating gas sensitive materials
Using absolute ethyl alcohol as adhesive, and mixing the prepared SnO2Mixing the powder sample with a certain amount of absolute ethyl alcohol solution to obtain butterfly-shaped two-dimensional structure SnO2And (3) fully grinding the nano material, and then mixing into paste for later use.
b. Sensitive material coating
The gas-sensitive material mixed into paste is uniformly coated on the surface of the ceramic tube with the prepared electrode to prepare a sensitive material layer, and the coating completely covers the gold electrode, and has proper thickness and uniform thickness.
c. Sintering of components
Drying the coated ceramic tube, placing the ceramic tube in a quartz boat, and sintering for 1-3 hours in a sintering furnace at the sintering temperature of 400-600 DEG CoC。
d. Wire bonding and packaging
And (4) placing a wound heating wire into the ceramic tube after sintering the ceramic plate. And then welding the electrode lead and the heating wire on the element base, and finishing the manufacturing of the sensor element.
e. Aging by electrical heating
The sensor element is placed in a special aging table, aging is carried out by a method of electrifying for 32-240 hours, and the aged element can be taken out to test the gas sensitive parameters.
The invention is further illustrated by the following specific examples:
first butterfly shaped SnO2Preparation of two-dimensional nano material and sensitivity to acetaldehyde gas
The preparation process is as described in the summary of the invention, and the preparation process flow is shown in figure 1.
Table 1 shows the preparation of butterfly-shaped SnO 23 examples of two-dimensional nanomaterials.
TABLE 1 butterfly-shaped SnO 23 implementation examples of two-dimensional nano material with various proportions
Butterfly-shaped SnO prepared in two or more than three embodiments2Examples of two-dimensional nanomaterial sensing Properties
1. Butterfly shaped SnO2Relationship between sensitivity of two-dimensional nano-material sensor to acetaldehyde and heating voltage
FIG. 8 is a butterfly-shaped SnO of the above three embodiments2The sensitivity of a sensor made of two-dimensional nano materials to 200ppm acetaldehyde is plotted against the heating voltage. Fig. 8 shows that the sensor has the highest sensitivity to acetaldehyde gas, which can reach 253, when the heating voltage is 2.5V. This illustrates butterfly-shaped SnO2The optimal heating voltage of the two-dimensional nano material sensor to acetaldehyde is very lowAnd illustrates a butterfly-shaped two-dimensional structure SnO2The gas sensitivity of the nano material changes along with the heat treatment temperature, which shows that the butterfly-shaped two-dimensional structure SnO can be realized by adjusting the heat treatment temperature2The modulation of the gas sensitivity performance of the nano material,
2. butterfly shaped SnO2Variation relation of sensitivity of two-dimensional nano material sensor along with concentration of acetaldehyde
FIG. 9 is a butterfly-shaped SnO of the above three embodiments2The sensitivity of the sensor made of the two-dimensional nano material is a curve of dynamic change along with the concentration of acetaldehyde when the heating voltage is 2.5V. As can be seen from FIG. 9, the butterfly-shaped two-dimensional structure SnO2The nanometer material has good reproducibility on the sensitivity of the acetaldehyde gas, and the sensitivity of the sensor is continuously and rapidly increased along with the increase of the concentration of the acetaldehyde gas. It is worth noting that the sensor has extremely high sensitivity to low concentrations of acetaldehyde, wherein the sensitivity to acetaldehyde gas at the 500 ppb level reaches 91.5, which well meets the need for detection of acetaldehyde at low concentrations. In addition, when the acetaldehyde concentration is 200-1000 ppm, the sensitivity of the sensor shows a good linear rapid increase relation along with the acetaldehyde concentration, which shows that the sensor has a wide detection range for the acetaldehyde gas.
Claims (6)
1. Butterfly-shaped SnO2Two-dimensional nanomaterials characterized in that said butterfly-shaped SnO2The two-dimensional nano material is SnSO4And SDBS as raw material, and is prepared by two steps of combining hydrothermal reaction and high-temperature oxidation annealing, wherein the SnO in the butterfly shape2The two-dimensional nano material has a two-dimensional butterfly shape and a rich surface defect structure, and the SnO of the butterfly shape2The size of each unit of the two-dimensional nano material is 15-80 mu m, the thickness of the lamella is 10-80 nm, and the rich surface defect structure is SnO with the butterfly shape of each unit2A plurality of protruding island-shaped surface defect structures grow on the surface, and the size of the island-shaped protrusions is 50 nm-2 mu m; the preparation method comprises the steps of precursor solution preparation, main reaction, precursor separation and nano material final preparation, and specifically comprises the following steps:
A. preparing a precursor solution:
1) accurately weighing sodium dodecyl benzene sulfonate, stirring and dissolving the sodium dodecyl benzene sulfonate into deionized water to prepare an aqueous solution with the molar concentration of 0.04-0.20 mol/L to obtain a solution a;
2) SnSO precision weighing4Adding the solution into the solution a, and stirring for 60-180 min to obtain a hydrothermal synthesis precursor reaction system b, wherein SnSO4The molar ratio of the SDBS to the SDBS is (1: 1) - (2: 1);
B. main reaction: heating the hydrothermal synthesis precursor reaction system b to 160-220 ℃ at the heating rate of 1-6 ℃/min, and then carrying out heat preservation reaction at 160-220 ℃ for 12-60 h to obtain a reaction solution c;
C. precursor separation: carrying out centrifugal separation on the reaction liquid c at the temperature below 4 ℃, wherein the rotating speed of the centrifugal separation is 12000-15000 r/min, and obtaining a hydrothermal reaction deposition product, namely a butterfly-shaped SnO precursor d;
D. preparing a nano material:
1) cleaning the butterfly-shaped SnO precursor d to remove reaction residues and reaction byproducts, and separating and drying to obtain a material e;
2) heating the material e to 550-800 ℃ at the heating rate of 2-5 ℃/min, preserving the heat for 60-120 min, and then cooling to normal temperature at the cooling rate of 2-5 ℃/min to obtain the target butterfly-shaped SnO2Two-dimensional nanomaterials.
2. The butterfly-shaped SnO of claim 12The two-dimensional nano material is characterized in that a vessel of the main reaction in the step B is a reaction kettle with a polytetrafluoroethylene lining.
3. The butterfly-shaped SnO of claim 12The two-dimensional nano material is characterized in that acetone, deionized water and absolute ethyl alcohol are adopted for repeated cleaning in the step D1).
4. The butterfly-shaped SnO of claim 12Two-dimensional nanomaterials, characterized in that the separation in step D1) is carried out through a 100 mesh sieveAnd (5) line filtering.
5. The butterfly-shaped SnO of claim 12The two-dimensional nano material is characterized in that the drying in the step D1) is carried out for 12-24 hours at the temperature of 60-80 ℃.
6. A butterfly shaped SnO according to claim 12The application of the two-dimensional nano material in preparing an acetaldehyde gas sensor.
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| CN110299423B (en) * | 2019-06-20 | 2020-11-13 | 浙江大学 | P-type two-dimensional alloy compound semiconductor photoelectric field effect transistor and preparation method thereof |
| CN110282654A (en) * | 2019-07-30 | 2019-09-27 | 云南大学 | A kind of pentagonal pyramid shape SnO2The preparation method and application of nano-array composite hierarchical structure tectosome nano material |
| US20220259062A1 (en) * | 2019-09-26 | 2022-08-18 | Lg Chem, Ltd. | Tin Oxide Forming Composition |
| CN110697763B (en) * | 2019-10-21 | 2022-03-04 | 云南大学 | Self-supporting SnO2Preparation method and application of nanorod ordered array material |
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