CN113880132A - Nitrogen-doped tin dioxide material with 3DOM structure and preparation method and application thereof - Google Patents
Nitrogen-doped tin dioxide material with 3DOM structure and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nitrogen-doped tin dioxide material with a 3DOM structure, and a preparation method and application thereof. Firstly, mixing silicon dioxide and dicyandiamide, then carrying out high-temperature calcination to obtain a compound of the silicon dioxide and carbon nitride, and then washing the silicon dioxide in the compound by using a sodium hydroxide solution to obtain pure carbon nitride. And then uniformly mixing the carbon nitride, the tin source material and the deionized water, drying, and calcining at a high temperature to obtain the nitrogen-doped tin dioxide with the 3DOM structure. The porous tin dioxide prepared by the method has the aperture of about 400nm and rich oxygen defects. The invention can effectively improve the specific surface area of the material, and regulate and control the electronic structure and the surface oxygen vacancy defect of the material, thereby obviously improving the NO of the material2The gas sensitivity performance of the gas sensor can further realize high response, low temperature response and lower detection lower limit to target gas.
Description
Technical Field
The invention relates to the technical field of gas-sensitive materials, in particular to a nitrogen-doped tin dioxide material with a 3DOM structure, a preparation method thereof and NO2Gas sensitive detection applications.
Background
Along with the current workersThe rapid development of industrialization brings great convenience to the life of people, the quality and level of life of people are continuously improved, but various environmental problems are also followed, the emission of automobile exhaust is more serious along with the increasing number of automobiles, and the automobile exhaust contains a large amount of NO2Seriously harming the environment and the health of people. NO2In addition to natural sources, mainly from fuel combustion and NO emissions from automobile exhaust2Can damage the respiratory tract of people, and cause chronic respiratory inflammation and neurasthenia syndrome. NO2Also, one of the causes of acid rain is the formation of various environmental effects, which seriously damage the ecological environment.
Semiconductor type gas sensors have been widely used for detecting toxic and harmful gases, and there have been many methods for detecting NO2But has the defects of insufficient detection capability, too high working temperature, limited detection limit and the like, and NO is detected at room temperature2Especially low concentration of NO2The detection of (2) is still an urgent problem to be solved. The method for improving the specific surface area of the material by regulating and controlling the shape and combining precious metals, metal oxides and the like to realize material doping and construct a heterostructure is a common gas-sensitive performance regulating and controlling method. Work by Dipyaman Mohanta et al on Sensors and actors B Chemical 326(2021)128910 showed loading of metallic Ag nanoparticles on SnO2And g-C3N4Can be carried out at room temperature to NO2And detection of NO2But at room temperature, the sensor pair NO2The responsivity of (2) is only a few tenths. A study by Liang et al on ACS Appl. Mater. Interfaces 2021,13,31968-31977 showed VO2For 5ppm NO in the case of UV irradiation2Has a responsivity of greater than 2. The sensor consumes more power when working at high temperature, and the noble metal doping is also very high in manufacturing cost, which is not favorable for realizing wide commercial application. Achieving room temperature detection and high responsiveness simultaneously remains a major challenge. Therefore, research and design can be performed at room temperature and can be realizedHigh-responsivity semiconductor gas-sensitive sensing material and gas-sensitive performance regulation method thereof for realizing low-concentration NO2The high-sensitivity and low-power consumption detection of the gas has important significance.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a nitrogen-doped tin dioxide material with a 3DOM structure, a preparation method thereof and NO2Gas sensitive detection applications. The invention can realize effective regulation and control of an electronic structure, improve the gas-sensitive response capability of the material, and realize high responsiveness, low detection temperature and low test limit detection of target gas.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a nitrogen-doped tin dioxide material with a 3DOM structure, which comprises the following steps:
(1) dissolving a tin source into deionized water to obtain a solution A; ultrasonically dispersing a 3DOM carbon nitride precursor in deionized water to obtain a solution B; adding the solution B into the solution A under stirring, and then continuing stirring at room temperature to obtain a carbon nitride-tin source mixture;
(2) and (2) washing, centrifuging and drying the carbon nitride-tin source mixture obtained in the step (1), calcining the dried product, and cooling to obtain the nitrogen-doped tin dioxide material with the 3DOM structure.
Preferably, in step (1), the 3DOM carbon nitride precursor is prepared by the following method:
a. uniformly mixing silicon dioxide, dicyandiamide and deionized water, then stirring, and centrifuging and drying after stirring;
b. and calcining the dried powder, uniformly mixing and stirring the calcined material and a sodium hydroxide solution, centrifuging, and drying to obtain the 3DOM carbon nitride precursor.
Preferably, in the step a, the adding amount ratio of the silicon dioxide, the dicyandiamide and the deionized water is 3 g: 6 g: 100 mL; the stirring temperature is 70 ℃ and the stirring time is 12 h.
Preferably, in the step b, the temperature rise rate of the calcination is 2.5 ℃/min, the calcination temperature is 550 ℃, and the calcination time is 3-5 h; the ratio of the addition of calcined material to sodium hydroxide solution was 1 g: 100mL, wherein the concentration of the sodium hydroxide solution is 1 mol/L; the stirring time is 10-15 h.
Preferably, in the step (1), the ratio of the added tin source to the added deionized water is (10-12) g: 10 mL; the adding amount ratio of the 3DOM carbon nitride precursor to the deionized water is (0.3-0.5) g: 10 mL; the tin source is selected from stannous chloride or stannous chloride pentahydrate; the stirring time at room temperature was 24 h.
Preferably, in the step (2), the carbon nitride-tin source mixture is washed by using deionized water and absolute ethyl alcohol alternately; the calcining temperature is 500 ℃, the heating rate is 2-10 ℃/min, and the calcining time is 1.5-2.5 h.
Preferably, the heating rate is 2 ℃/min, 5 ℃/min or 10 ℃/min.
In a second aspect of the invention, the nitrogen-doped tin dioxide material with the 3DOM structure is obtained by the preparation method, and the nitrogen-doped tin dioxide material with the 3DOM structure is rich in oxygen vacancy defects.
Preferably, the aperture size of the nitrogen-doped tin dioxide material with the 3DOM structure is 300-500 nm.
In a third aspect of the invention, the nitrogen-doped tin dioxide material with the 3DOM structure is provided for preparing NO2Gas sensor or detecting NO2The use of (1).
The invention has the beneficial effects that:
1. the invention provides a nitrogen-doped tin dioxide material with a 3DOM structure, a preparation method thereof and application of the material in NO2And (5) detecting gas. Compared with the traditional semiconductor gas-sensitive material, the composite material prepared by the method has the advantage of large specific surface area of the porous material. In addition, most of the porous carbon and nitrogen are burnt out through high-temperature calcination, a small amount of amorphous carbon and nitrogen are reserved, the carbon and nitrogen doping of tin dioxide is realized, a large amount of surface oxygen defects are generated in the calcination process, more surface oxygen can be adsorbed, and the surface oxygen reacts with more target gas molecules to generate the tin dioxideA higher response is generated.
2. The nitrogen-doped tin dioxide material with the 3DOM structure prepared by the invention is used for a gas sensor, and NO can be treated at room temperature2Gas detection, and can realize extremely high response capability to 10ppm NO at room temperature2The gas responsivity was 930 and the detection limit was 18.5 ppb.
3. The gas-sensitive sensing material prepared by the invention has simple preparation process, is convenient for batch production, has high repeatability, and meets the requirements of high sensitivity and low working temperature NO on the current market2The demand for gas sensors.
Drawings
FIG. 1 is a transmission electron micrograph (a) and a high magnification view (b) of a 3 DOM-structured nitrogen-doped tin dioxide material prepared in example 1.
FIG. 2 shows the X-ray diffraction pattern and standard SnO of the 3 DOM-structured nitrogen-doped tin dioxide materials prepared in examples 1 and 22The spectrogram PDF #41-1445 is aligned with the card.
Fig. 3 is a high resolution lattice diagram (a) and elemental surface scan diagram (b) of the 3DOM structured nitrogen-doped tin dioxide material prepared in example 1.
FIG. 4 is the O element spectrum in the X-ray photoelectron spectrum of the nitrogen-doped tin dioxide material of 3DOM structure in example 2: (a) NS-1; (b) NS-2; (c) NS-3.
Fig. 5 is the responsivity of the 3DOM structured nitrogen doped tin dioxide material prepared in examples 1 and 2 to gases such as nitrogen dioxide, ammonia, hydrogen, carbon monoxide, hydrogen sulfide and ethanol.
Figure 6 is a graph of the responsivity as a function of concentration of nitrogen dioxide for nitrogen dioxide at room temperature for the 3 DOM-structured nitrogen-doped tin dioxide prepared in examples 1 and 2: (a) NS-1; (b) NS-2; (c) NS-3.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background section, the prior art gas sensitive sensing material is sensitive to NO2The detection of (2) needs to be performed at a higher operating temperature. The current research work still has difficulty in combining low working temperature and high response capability, the overhigh working temperature brings larger power consumption, and the price of the noble metal is overhigh, which limits the application of the noble metal in NO2The method is widely applied to detection.
Based on the above, the invention provides a nitrogen-doped tin dioxide material with a 3DOM structure, a preparation method thereof and NO2Gas sensitive detection applications. Firstly, mixing silicon dioxide and dicyandiamide, then obtaining a compound of the silicon dioxide and carbon nitride through a high-temperature calcination process, and then washing the silicon dioxide in the compound by using a sodium hydroxide solution to obtain pure carbon nitride. And then uniformly mixing the carbon nitride, the tin source material and the deionized water, drying, and calcining at a high temperature to obtain the nitrogen-doped tin dioxide with the 3DOM structure. Meanwhile, the invention also finds that the adjustment of the oxygen vacancy defect concentration on the surface of the material can be realized by controlling the temperature rise rate in the calcining process. The method comprises the steps of adsorbing a tin source by using carbon nitride with a 3DOM structure, and then burning off part of carbon and nitrogen by calcining to form a small amount of carbon and nitrogen-doped tin dioxide with the 3DOM structure. The reserved small amount of amorphous carbon nitrogen can improve the conductivity of the material and improve the gas-sensitive performance of the material.
The nitrogen-doped tin dioxide material has a porous structure, and the distribution of pores is uniform. Compared with the common tin dioxide material, the tin dioxide material has larger specific surface area, so that the material has more reaction sites, more gas molecules are in full contact with the material and react, and higher response is generated. In addition, in the preparation process of the material, the concentration of oxygen vacancy defects on the surface of the material can be effectively regulated and controlled by the difference of the heating rates in the high-temperature calcination process, and the material can generate more oxygen vacancy defects along with the continuous acceleration of the heating rate, so that more surface free electrons and surface adsorbed oxygen are provided, and the detection of high responsiveness, low detection temperature and low test limit of target gas is realized.
The invention can effectively improve the detection capability of the gas sensitive material on the target gas by constructing the surface oxygen defect. Oxygen defects can introduce a large number of unsaturated metal atoms, thereby providing more surface free electrons and increasing the electronic state near the fermi level, providing more surface adsorbed oxygen at the material surface. The method can realize effective regulation and control of the electronic structure, improve the gas-sensitive response capability of the material, and realize high responsiveness, low detection temperature and low detection limit detection of the target gas.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and commercially available.
Example 1: nitrogen-doped tin dioxide material with 3DOM structure and preparation method thereof
(1) Preparation of porous carbon nitride
Fully mixing 3g of silicon dioxide, 6g of dicyandiamide and 100mL of deionized water, carrying out ultrasonic treatment for 2 hours in an ultrasonic cleaning machine with the frequency of 40KHz and the power of 400W, stirring for 12 hours at 70 ℃, centrifuging in a centrifuge with the rotating speed of 8000rpm/min after fully stirring, and carrying out drying treatment for 24 hours in a vacuum drying oven at 60 ℃. And (3) calcining the collected powder at high temperature, and calcining at 550 ℃ at the heating rate of 2.5 ℃/min. And (2) fully mixing 1g of calcined material with 100mL of 1moL/L sodium hydroxide solution, stirring for 10-15 hours at room temperature, carrying out ultrasonic treatment in an ultrasonic cleaning machine with the frequency of 40KHz and the power of 400W for multiple times, centrifuging in a centrifuge with the rotating speed of 8000rpm/min, and drying for 24 hours in a vacuum drying oven at the temperature of 60 ℃ to obtain pure porous carbon nitride.
(2) Preparation of nitrogen-doped tin dioxide material with porous structure
(2.1) Add 11.4g stannous chloride to 10mL deionized water and stir well at room temperature until well dissolved to give solution A.
(2.2) taking 0.4g of the porous carbon nitride prepared in the step (1), adding 10mL of deionized water, carrying out ultrasonic treatment for 15 minutes in an ultrasonic cleaner with the frequency of 40KHz and the power of 400W, and fully stirring at room temperature to obtain a solution B.
(2.3) while stirring solution A, solution B was slowly poured into solution A, and stirring was continued at room temperature for 24 hours. After stirring was complete, the well mixed solution was centrifuged and vacuum dried at 60 ℃ for 24 hours and the powder material was collected. And (3) calcining the collected material at high temperature, wherein the calcining temperature is 500 ℃, the calcining time is 2 hours, and the heating rate is 2 ℃ per minute. After the calcination is finished, the nitrogen-doped tin dioxide material (named NS-1) with a 3DOM structure is obtained.
As shown in fig. 1, the nitrogen-doped tin dioxide material having a porous structure prepared using example 1 exhibited a significant porous structure with a pore size of 400 nm. As shown in fig. 2, it can be seen from the X-ray diffraction pattern that the respective peak positions of the material can be matched with the standard spectrum of tin dioxide, and thus, it can be confirmed that the tin source material has been completely changed into tin dioxide after high-temperature calcination. Furthermore, it can be seen from fig. 3 that tin dioxide not only realizes a porous structure, but also realizes carbon and nitrogen doping.
Example 2: oxygen vacancy defect regulation and control method of nitrogen-doped tin dioxide material with 3DOM structure
The difference between this example and example 1 is that in step (2.3), the temperature rise rate during the high-temperature calcination process was adjusted from 2 ℃/min to 5 ℃/min and 10 ℃/min, respectively, and the remaining steps were the same as example 1, and the obtained materials were named NS-2 and NS-3, respectively.
The concentration of oxygen vacancy defects on the surface of the material is regulated and controlled by controlling the temperature rise rate in the high-temperature calcination process. As shown in FIG. 4, oxygen vacancy defects O varied with the temperature increase rateovThe proportion of the O1s spectrum also changes. The number of oxygen vacancy defects increases significantly as the rate of temperature rise increases.
Example 3: nitrogen-doped tin dioxide material NO with 3DOM structure2Gas sensitive detection applications
(1) The nitrogen-doped tin dioxide material with the 3DOM structure prepared in the example 1-2 comprises: NS-1, NS-2 and NS-3 are respectively mixed with absolute ethyl alcohol to form slurry, and the slurry is placed in an ultrasonic disperser to be dispersed for 10 minutes, so that the particle agglomeration is reduced.
(2) Applying a uniform gas-sensitive paste to Al with electrodes at both ends2O3And (5) drying the ceramic tube naturally to obtain the gas sensor with uniform coating. And placing the obtained gas sensor on a gas-sensitive aging table, and aging for 5 days at 200 ℃.
(3) And (3) placing the gas sensor prepared in the step (2) on a WS-30A gas-sensitive test platform, supplying power by using 5V voltage, introducing a load card as a protection resistor of a circuit, and leading out an output voltage characteristic curve of a gas sensor load on a computer to be converted into a characteristic curve of the resistor, wherein the concentration of the gas to be measured can be reflected through the variation intensity of the resistor. The NS-1, NS-2, NS-3 sensors are subjected to gas-sensitive performance test at room temperature, and NO of each sensor is respectively detected2、NH3、H2、CO、H2S and ethanol, etc.
As shown in FIG. 5, NS-3 sensor is paired with NO2The gas showed the best gas sensitive response to 10ppm NO at room temperature2The gas response reaches 926 and is far higher than NO of other sensors2Gas sensitive response capability. The working temperature is room temperature, the power consumption of the sensor is also reduced, and the sensor is beneficial to NO2Practical application in the detection field.
(4) Testing NO of each gas sensor in the step (3) when the working temperature of each gas sensor is room temperature2The responsivity of (A) is changed with the concentration (1-10 ppm). As shown in FIG. 6, each sensor pair has NO with increasing concentration2The responsivity of (a) is continuously enhanced. In addition, NS-3 sensor pairs NO2The responsivity of the gas is higher than other sensors throughout the concentration range. Exhibit excellent NO2Gas sensing performance.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. A preparation method of a nitrogen-doped tin dioxide material with a 3DOM structure is characterized by comprising the following steps:
(1) dissolving a tin source into deionized water to obtain a solution A; ultrasonically dispersing a 3DOM carbon nitride precursor in deionized water to obtain a solution B; adding the solution B into the solution A under stirring, and then continuing stirring at room temperature to obtain a carbon nitride-tin source mixture;
(2) and (2) washing, centrifuging and drying the carbon nitride-tin source mixture obtained in the step (1), calcining the dried product, and cooling to obtain the nitrogen-doped tin dioxide material with the 3DOM structure.
2. The method according to claim 1, wherein in step (1), the 3DOM carbon nitride precursor is prepared by:
a. uniformly mixing silicon dioxide, dicyandiamide and deionized water, then stirring, and centrifuging and drying after stirring;
b. and calcining the dried powder, uniformly mixing and stirring the calcined material and a sodium hydroxide solution, centrifuging, and drying to obtain the 3DOM carbon nitride precursor.
3. The preparation method according to claim 2, wherein in the step a, the ratio of the added amounts of the silicon dioxide, the dicyandiamide and the deionized water is 3 g: 6 g: 100 mL; the stirring temperature is 70 ℃ and the stirring time is 12 h.
4. The preparation method of claim 2, wherein in the step b, the temperature rise rate of the calcination is 2.5 ℃/min, the calcination temperature is 550 ℃, and the calcination time is 3-5 h; the ratio of the addition of calcined material to sodium hydroxide solution was 1 g: 100mL, wherein the concentration of the sodium hydroxide solution is 1 moL/L; the stirring time is 10-15 h.
5. The method according to claim 1, wherein in the step (1), the ratio of the added amount of the tin source to the added amount of the deionized water is (10-12) g: 10 mL; the adding amount ratio of the 3DOM carbon nitride precursor to the deionized water is (0.3-0.5) g: 10 mL; the tin source is selected from stannous chloride or stannous chloride pentahydrate; the stirring time at room temperature was 24 h.
6. The production method according to claim 1, wherein in the step (2), the washing is: alternately washing the carbon nitride-tin source mixture with deionized water and absolute ethyl alcohol; the calcining temperature is 500 ℃, the heating rate is 2-10 ℃/min, and the calcining time is 1.5-2.5 h.
7. The method according to claim 6, wherein the temperature increase rate is 2 ℃/min, 5 ℃/min, or 10 ℃/min.
8. The nitrogen-doped tin dioxide material with the 3DOM structure obtained by the preparation method of claims 1-7, wherein the nitrogen-doped tin dioxide material with the 3DOM structure is rich in oxygen vacancy defects.
9. The 3DOM structured nitrogen doped tin dioxide material of claim 8, wherein the 3DOM structured nitrogen doped tin dioxide material has a pore size of 300 to 500 nm.
10. Use of the 3DOM structured nitrogen-doped tin dioxide material of claim 8 or 9 in the preparation of NO2Gas sensor or detecting NO2The use of (1).
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