CN111484071A - SnO with amorphous/crystalline structure on surface2Synthesis method of material and photocatalytic application thereof - Google Patents

SnO with amorphous/crystalline structure on surface2Synthesis method of material and photocatalytic application thereof Download PDF

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Publication number
CN111484071A
CN111484071A CN202010135506.9A CN202010135506A CN111484071A CN 111484071 A CN111484071 A CN 111484071A CN 202010135506 A CN202010135506 A CN 202010135506A CN 111484071 A CN111484071 A CN 111484071A
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sno
reaction
amorphous
crystalline structure
drying
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张荔
同若冰
杨艳玲
侯小江
冯雷
锁国权
叶晓慧
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/02—Oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8628—Processes characterised by a specific catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
    • B01J35/39—
    • B01J35/51—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B01D2257/404—Nitrogen oxides other than dinitrogen oxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/06—Polluted air
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer

Abstract

SnO with amorphous/crystalline structure on surface2The synthesis method of the material and the photocatalytic application thereof comprise the following steps: SnCl2Dispersing the tin source in a solvent, and dissolving the tin source by ultrasonic waves; step two: transferring the solution obtained in the first step into a polytetrafluoroethylene reaction kettle of a reaction kettle, putting the reaction kettle into a drying oven for reaction, and heating to the temperature required by the reaction for heat preservation; step three: naturally cooling to room temperature after the reaction is finished, collecting the obtained product, centrifugally cleaning, and drying to obtain light yellow powder and obtain SnO with uniform size2A micron-spherical material. The invention is provided withAnhydrous ethanol as solvent, SnCl2Is a tin source, is reacted in a high-temperature reaction kettle, and SnO with uniform particle size is grown through three stages of temperature rise, heat preservation and temperature reduction2The micron spheres provide a larger specific surface area for photocatalytic reaction.

Description

SnO with amorphous/crystalline structure on surface2Synthesis method of material and photocatalytic application thereof
Technical Field
The invention relates to the technical field of metal oxide materials, in particular to SnO with an amorphous/crystalline surface structure2A method for synthesizing the material and the application of photocatalysis.
Background
NO is a typical component in air pollutants in some countries in the world, and the removal of NO is of great significance for air purification. Various methods such as physical/chemical adsorption, selective catalytic reduction, thermocatalytic reduction have been developed for the removal of NO. Photocatalytic removal of low concentrations of NO is one of the most promising approaches, since it can directly utilize solar energy without introducing additional energy sources. For decades, TiO has been used2、Bi2O2CO3、Bi2WO6、C3N4、Bi2O3Various semiconductors are studied for photocatalytic removal of NO, and found to have excellent catalytic activity. However, many of these semiconductors do not completely oxidize NO to Nitrate (NO)3 -) Often nitrogen dioxide (NO) is obtained2)，NO2Compared with NO, the product has higher toxicity. SnO2The N-type semiconductor has a band gap of 3.60eV, high chemical stability and excellent electronic and optical properties, and is widely applied to the fields of gas sensors, photochemistry, photodetectors and the like. In the field of photocatalysis, with commercial materials TiO2In contrast, SnO2Has stronger valence band and oxidation capability, and is expected to oxidize pollutants more thoroughly. However, since SnO2The inherent wide bandgap properties (3.60eV) make it very limited to use visible light in photocatalysis. Currently improving photocatalysisThe performance of the material is mainly realized by doping or constructing a heterojunction and the like. The invention improves SnO by constructing a special surface amorphous/crystalline structure2The photocatalytic performance of the material is mainly achieved by introducing an amorphous structure to increase oxygen vacancies, introducing more active sites, constructing homojunctions to form a built-in electric field, providing a driving force for charge transmission, accelerating the separation of photo-generated charges and further improving the photocatalytic performance.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide SnO with an amorphous/crystalline surface structure2The material is synthesized with anhydrous alcohol as solvent and SnCl as catalyst2Is a tin source, is reacted in a high-temperature reaction kettle, and SnO with uniform particle size is grown through three stages of temperature rise, heat preservation and temperature reduction2The micron spheres provide a larger specific surface area for photocatalytic reaction.
In order to achieve the purpose, the invention adopts the technical scheme that:
SnO with amorphous/crystalline structure on surface2A method for synthesizing a material, comprising the steps of;
the method comprises the following steps: SnCl2Dispersing the tin source in a solvent, and dissolving the tin source by ultrasonic waves;
step two: transferring the solution obtained in the first step into a polytetrafluoroethylene reaction kettle of a reaction kettle, putting the reaction kettle into a drying oven for reaction, and heating to the temperature required by the reaction for heat preservation;
step three: naturally cooling to room temperature after the reaction is finished, collecting the obtained product, centrifugally cleaning, and drying to obtain light yellow powder and obtain SnO with uniform size2A micron-spherical material.
SnCl in the step one2The mass is 1.8g, the solvent is absolute ethyl alcohol, the volume is 30-40m L, and the ultrasonic time is 0.5-1 h.
The reaction temperature in the second step is 180-220 ℃, and the reaction time is 5-7 hours.
And in the second step, 70-80% of the filling amount of the inner liner is calculated according to the volume of the inner liner.
The third step is that the faint yellow powder is SnO2。
The third step of centrifugal cleaning and drying conditions are that the mixture is cleaned by absolute ethyl alcohol, centrifuged and dried for 3 hours at 60 DEG C
Said SnO2The surface of the micron spherical material is composed of crystalline and amorphous structures alternately.
Said SnO2The micron spherical material is a uniform spherical material with the diameter of 2-3 microns.
Said SnO2The micron spherical material is applied to photocatalysis, is used for removing NO in a photocatalysis material, and specifically is prepared by using faint yellow powder SnO2Ultrasonically dispersing the micron spherical material in water, transferring the micron spherical material into a watch glass, and drying to obtain SnO2And (4) carrying out a photocatalytic reaction, and putting the watch glass containing the sample into a quartz reaction chamber for carrying out the photocatalytic reaction.
Said SnO2The mass of the micron spherical material is 30-50mg, the volume of water is 10-15m L, the ultrasonic time is 15-20 minutes, the drying temperature is 60-70 ℃, and the drying time is 3-5 hours.
The invention has the beneficial effects that:
the whole involved operation process is convenient and simple, the liquid generated by the reaction only needs to be cleaned by ethanol after centrifugation, and the method does not involve any acid washing process and has no pollution to the environment.
The synthesis method adopted by the experiment is simple, convenient, efficient, safe and harmless, the time of the whole experiment process is short, and the repeatability is high. The experiment uses a simple one-step solvothermal method, and synthesizes SnO with an amorphous/crystalline structure by adjusting reaction time2The spherical micron particles provide more surface oxygen defects and active sites for the material, reduce the forbidden bandwidth of the material, improve the utilization rate of a visible light range, and reduce the recombination rate of photon-generated carriers by a generated surface electric field so as to improve the photocatalytic efficiency. SnO2The mechanism of the photocatalytic removal of NO is SnO under the condition of illumination2The valence electron is excited to transition from the valence band to the conduction band, leaving a hole in the valence band. Photoelectrons and holes with adsorbed O2And H2O reacts to form superoxide radicals and hydroxyl radicals as the active species for the removal of NO.
Said SnO2The surface of the micron spherical material is composed of crystalline and amorphous structures alternately, rich oxygen vacancy defects are formed at the same time, and the effect of removing NO by photocatalysis is obviously enhanced.
The invention takes absolute ethyl alcohol as solvent and SnCl2Is a tin source, is reacted in a high-temperature reaction kettle, and SnO with uniform particle size is grown through three stages of temperature rise, heat preservation and temperature reduction2The particle size of the micro-spheres is about 2-3 mu m, and a larger specific surface area is provided for photocatalytic reaction.
Drawings
FIG. 1 shows example 1 with two commercially available SnO2XRD pattern of (a).
FIG. 2 shows example 1 with two commercially available SnO2SEM photograph of (a).
FIG. 3 is SnO in example 12TEM photograph of (a).
FIG. 4 is SnO in example 12With two commercially available SnO2Comparative plot of the photocatalytic NO removal efficiency.
FIG. 5 shows example 1 with two commercially available SnO2UV-vis spectrum of (1).
FIG. 6 shows example 1 with two commercially available SnO2An EPR map of (1).
FIG. 7 is SnO in example 12KPFM map of (a).
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
Weighing 1.8g SnCl2Dissolving in 30m L anhydrous ethanol, performing ultrasonic treatment for 30 min to completely dissolve, transferring the obtained colorless transparent solution into a polytetrafluoroethylene reaction kettle, placing into an oven, heating to 220 deg.C, keeping the temperature for 6 hr, naturally cooling to room temperature, collecting the obtained reactant, washing with anhydrous ethanol, centrifuging, drying at 60 deg.C for 3 hr to obtain yellowish SnO2And (3) powder.
Will be synthesizedSnO2Powder and two commercially available snos2The powders are respectively named SnO2、 SnO2-1 and SnO2-2。
FIG. 1 is a schematic representation of three SnO species2X-ray diffraction pattern (XRD) of the powder, all diffraction peaks are equal to SnO2Standard card (PDF #04-003-2The powder is pure phase. Synthesis of SnO2The powder has wider XRD diffraction peak, which indicates that the synthesized SnO2The crystallinity of the powder is low.
SEM photograph of FIG. 2 shows synthesized SnO2The powder is spherical with the diameter of 2-3 mu m and has a nano concave pit and nano convex structure with gully-shaped surface.
TEM photograph of FIG. 3 shows synthesized SnO2The micro-sphere is formed by self-assembly growth of nano small crystal grains, a nano pit is formed on the contact surface of the nano crystal grains, the lattice stripes are disordered, the internal lattice stripes of the nano crystal grains are very regular, and the amorphous nano pit and the crystalline bulge jointly form an amorphous/crystalline structure SnO2A material.
FIG. 4 is a graph of three SnO species2The NO removal efficiency chart of the powder by photocatalysis shows that the synthesized SnO2The degradation efficiency of the powder to NO is two kinds of commercially available SnO24-5 times of the total weight of the product.
FIG. 5 is a schematic of three SnO2Ultraviolet spectrum of the powder is compared with two commercially available SnO2Powder, synthesized SnO2The powder has obviously enhanced absorption intensity in a visible light region, and the absorption edge generates red shift, which shows that the powder has stronger activity of removing NO by photocatalysis.
FIG. 6 is a schematic of three SnO2EPR spectrum of the powder, paramagnetic center is at 2.003, compared with two kinds of SnO sold in the market2Powder, synthetic SnO2The powder illustrates the presence of a large number of oxygen vacancies at the surface of the synthesized dioxides.
FIG. 7 is a diagram of synthetic SnO2KPFM spectrum (material surface height and surface potential diagram) of the powder shows that larger potential difference exists between nano concave and convex structures existing on the surface of the powder at the same time, and confirms that the amorphous concave and the crystalline convex existThere is an electric field in between.
SnO2The surface of the micron spherical material is composed of crystalline and amorphous structures alternately, rich oxygen vacancy defects are formed simultaneously, and the effect of removing NO by photocatalysis is obviously enhanced.
SnO prepared by the method2The micron spherical material is a uniform spherical material with the diameter of 2-3 microns.
SnO prepared by the method2The application of the micron spherical material in removing NO by the photocatalytic material.
SnO prepared by the method2The performance of the micron spherical material for removing NO by photocatalysis is that two kinds of SnO sold in the market2(purity 99.8% by national drug control stock Co., Ltd.; purity 99.5% by Aladdin Co., Ltd.) as a comparative sample.
Example 2
Weighing 1.8g SnCl2Dissolving in 30m L anhydrous ethanol, performing ultrasonic treatment for 30 min to completely dissolve, transferring the obtained colorless transparent solution into a polytetrafluoroethylene reaction kettle, placing into an oven, heating to 200 deg.C, keeping the temperature for 6 hr, naturally cooling to room temperature, collecting the obtained reactant, washing with anhydrous ethanol, centrifuging, drying at 60 deg.C for 3 hr to obtain yellowish SnO2And (3) powder.
Example 3
Weighing 1.8g SnCl2Dissolving in 30m L anhydrous ethanol, performing ultrasonic treatment for 30 min to completely dissolve, transferring the obtained colorless transparent solution into a polytetrafluoroethylene reaction kettle, placing into an oven, heating to 220 deg.C, keeping the temperature for 5 hr, naturally cooling to room temperature, collecting the obtained reactant, washing with anhydrous ethanol, centrifuging, drying at 60 deg.C for 3 hr to obtain yellowish SnO2And (3) powder.
The invention provides SnO for constructing an amorphous/crystalline structure2The material synthesis method is applied to the field of NO removal by photocatalysis. The special structure of the surface is SnO2The material provides more oxygen vacancies, so that the forbidden bandwidth of the material is reduced, the material is easier to be excited by visible light, and simultaneously, the generated surface electric field reduces the recombination efficiency of photo-generated hole electron pairs and generates more reactive active species(e.g., superoxide radical, hydroxyl radical), thereby increasing the efficiency of photocatalytic NO removal.
For further research the institute of SnO synthesis2Defects and electronic structures in the Material two commercially available SnO2Materials as a comparative study, all samples were analyzed for their light absorption capacity by ultraviolet-visible spectrophotometer (UV-vis), FIG. 4, and the synthetic SnO was found experimentally2The sample shows strong absorption in the ultraviolet region and also has obvious absorption in the visible light range of 600-800nm, but the two commercial samples have no obvious absorption in the visible light range, so that the experimental synthesized SnO2The absorption in the visible light region is higher than that of two commercially available SnO2And (4) sampling. The forbidden band widths of the synthesized sample and two commercial samples are respectively 2.96eV, 3.73eV and 3.71eV, and the synthesized SnO2The forbidden band width of the sample is smaller than that of two commercially available samples, which is probably related to the fact that the surface amorphous structure of the synthesized sample contains a large number of oxygen vacancies, because the oxygen vacancies can reduce the band gap of the semiconductor to a defect level, so that the material is easier to be excited by visible light, and the Electron Paramagnetic Resonance (EPR) experiment result further shows that the synthesized SnO is synthesized2The sample surface contained a high concentration of oxygen vacancies (see fig. 5). Kelvin Probe Force Microscopy (KPFM) results show that synthetic SnO2The surface amorphous and crystalline regions of the material have potential difference, namely surface electric field, and the recombination efficiency of hole and electron is reduced by the presence of the surface electric field, so that compared with SnO reported in the literature2The efficiency of removing NO by photocatalysis, amorphous/crystalline SnO synthesized by the experiment2The material has higher efficiency of removing NO by photocatalysis (as shown in figure 3).

Claims (10)

1. SnO with amorphous/crystalline structure on surface2A method for synthesizing a material, comprising the steps of;
the method comprises the following steps: SnCl2Dispersing the tin source in a solvent, and dissolving the tin source by ultrasonic waves;
step two: transferring the solution obtained in the first step into a polytetrafluoroethylene reaction kettle of a reaction kettle, putting the reaction kettle into a drying oven for reaction, and heating to the temperature required by the reaction for heat preservation;
step three: naturally cooling to room temperature after the reaction is finished, collecting the obtained product, centrifugally cleaning, and drying to obtain light yellow powder and obtain SnO with uniform size2A micron-spherical material.
2. A surface amorphous/crystalline structure SnO according to claim 12The method for synthesizing the material is characterized in that SnCl in the step one2The mass is 1.8g, the solvent is absolute ethyl alcohol, the volume is 30-40m L, and the ultrasonic time is 0.5-1 h.
3. A surface amorphous/crystalline structure SnO according to claim 12The method for synthesizing the material is characterized in that the reaction temperature in the second step is 180-220 ℃, and the reaction time is 5-7 hours.
4. A surface amorphous/crystalline structure SnO according to claim 12The method for synthesizing the material is characterized in that in the second step, the filling amount is 70-80% of the filling amount of the volume of the lining.
5. A surface amorphous/crystalline structure SnO according to claim 12The synthesis method of the material is characterized in that the faint yellow powder in the third step is SnO2。
6. A surface amorphous/crystalline structure SnO according to claim 12The synthesis method of the material is characterized in that the conditions of centrifugal cleaning and drying in the third step are that the material is cleaned by absolute ethyl alcohol and then dried for 3 hours at 60 ℃.
7. A surface amorphous/crystalline structure SnO according to claim 12The synthesis method of the material is characterized in that the SnO2The surface of the micron spherical material is composed of crystalline and amorphous structures alternately.
8. According to claim1 said SnO with amorphous/crystalline surface structure2The synthesis method of the material is characterized in that the SnO2The micron spherical material is a uniform spherical material with the diameter of 2-3 microns.
9. The SnO of claim 12The micron spherical material is applied to photocatalysis, is used for removing NO in a photocatalysis material, and specifically is prepared by using faint yellow powder SnO2Ultrasonically dispersing the micron spherical material in water, transferring the micron spherical material into a watch glass, and drying to obtain SnO2And (4) carrying out a photocatalytic reaction, and putting the watch glass filled with the sample into a quartz reaction chamber for carrying out the photocatalytic reaction.
10. A SnO according to claim 92The micron spherical material is applied to photocatalysis and is characterized in that the SnO2The mass of the micron spherical material is 30-50mg, the volume of water is 10-15m L, the ultrasonic time is 15-20 minutes, the drying temperature is 60-70 ℃, and the drying time is 3-5 hours.
CN202010135506.9A 2020-03-02 2020-03-02 SnO with amorphous/crystalline structure on surface2Synthesis method of material and photocatalytic application thereof Pending CN111484071A (en)

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US20180008953A1 (en) * 2016-07-08 2018-01-11 Soochow University Composite with synergistic effect of adsorption and visible light catalytic degradation and preparation method and application thereof
US20190126243A1 (en) * 2017-10-27 2019-05-02 Soochow University Preparation method of a visible-light-driven cc@sns2/sno2 composite catalyst, and application thereof
CN109682867A (en) * 2019-01-23 2019-04-26 陕西科技大学 A kind of micron order tin dioxide gas-sensitive material and its preparation method and application
CN110773221A (en) * 2019-11-08 2020-02-11 燕山大学 SnO synthesized by electrostatic self-assembly method 2/2D g-C 3N 4Preparation method of composite photocatalyst

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Title
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YANZHAO ZOU ET AL.: ""SnO2 quantum dots anchored on g-C3N4 for enhanced visible-light photocatalytic removal of NO and toxic NO2 inhibition"", 《APPLIED SURFACE SCIENCE》, vol. 496, 10 August 2019 (2019-08-10), pages 4 - 5, XP085850107, DOI: 10.1016/j.apsusc.2019.143630 *
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