CN112062104A - In2Se3Application of quantum dots and preparation method thereof - Google Patents
In2Se3Application of quantum dots and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011941 photocatalyst Substances 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
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- 238000005119 centrifugation Methods 0.000 claims description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 4
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
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- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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Abstract
The invention discloses In-based2Se3Application method of quantum dot. The invention also discloses In2Se3The preparation method of the quantum dot comprises the following specific steps: in is formed by2Se3Taking crystal powder as raw material, and ultrasonically stripping In polar solvent to obtain In-containing2Se3The dispersion liquid of the quantum dots is firstly centrifuged at a low rotating speed, then supernatant liquid is taken, and then the quantum dots in the dispersion liquid are precipitated through high-speed centrifugation; washing the precipitate with absolute ethanol and drying at low temperature to obtain In2Se3Quantum dot powderAnd (3) grinding. In provided by the invention2Se3The preparation conditions of the quantum dots are simple and easy to operate, the cost is low, and the obtained In2Se3The quantum dots are uniform in size and have good biocompatibility. The present invention provides an In2Se3The quantum dots are applied to the field of dye degradation as a photocatalyst, and the effect is obvious. The composite photocatalyst of the invention provides more active sites due to the small size and reduces the recombination of photon-generated carriers, and the dye degradation rate can reach 48.9%.
Description
Technical Field
The present invention relates to In2Se3QuantumAn application of the spot and a preparation method thereof, in particular to the field of dye degradation.
Background
Nowadays, environmental pollution is a common problem facing the world, the photocatalytic degradation of pollutants by using semiconductors is the best method for solving the problem, and the selection of efficient and stable photocatalysts is the central importance of the process. Conventional photocatalyst TiO2Because the band gap is large, the material can only absorb ultraviolet light which accounts for 5% of solar radiation energy, and the carrier mobility is low, the recombination rate is high, and extra substances such as oxidant and the like need to be added when the material is used, so that the photocatalytic efficiency is seriously influenced. Therefore, the search for the development of a novel photocatalyst for efficient degradation is of great significance.
At present, the method for treating dye wastewater mainly comprises physical adsorption, chemical treatment and biological treatment. Physical adsorption has selectivity on the adsorption of soluble dyes, and high-concentration pollutants cannot be treated; the chemical treatment may cause secondary pollution, and the cost is high; the biological treatment mainly depends on fungi and bacteria, and has selectivity to the dye, long culture colony period and high cost. Therefore, the catalyst which can be recycled by utilizing visible light to carry out photocatalytic degradation on the dye is found to have practical application and potential application prospect.
Conventional photocatalyst TiO2Due to the large band gap, the photocatalyst can only absorb ultraviolet light accounting for 5% of solar radiation energy, and has low carrier mobility and high recombination rate, thereby seriously affecting the photocatalytic efficiency. In2Se3The composite material has the advantages of small band gap, strong absorption on ultraviolet-visible light wave bands, high carrier mobility and ultrathin property, can reduce the recombination rate of photo-generated electrons and holes, provides a large number of potential reaction active sites with large specific surface area, can improve the photocatalytic performance, and shows good photocatalytic performance in previous researches.
Disclosure of Invention
The invention aims to overcome the defects of the existing photocatalyst and provide In2Se3Application of quantum dots and a preparation method thereof. The method utilizes a liquid phase stripping method to prepare In with uniform shape and controllable particle size on a large scale2Se3Quantum dots obtained by centrifugal drying of In2Se3Quantum dot powder, and In is provided2Se3Application of quantum dots in dye degradation.
In2Se3The quantum dots are applied specifically to In2Se3And carrying out photocatalytic degradation on the dye by using the quantum dots.
Wherein, In2Se3The size of the quantum dots is less than or equal to 5 nm.
The technical solution for realizing the above purpose of the invention is as follows:
performing ultrasonic treatment for 6h at power of 450W and 600W in polar solvent by liquid phase stripping method, centrifuging for 20min at 7000rmp/min to obtain quantum dot supernatant, and centrifuging for 30min at centrifugation rate of 10000rmp/min to precipitate quantum dots in the solution; the precipitate was washed 3 times with absolute ethanol and dried at low temperature of 40 ℃ for weighing.
Wherein the polar solvent comprises at least one of water, ethanol, isopropanol, and N-methylpyrrolidone
Compared with the prior art, the invention has the following remarkable advantages:
the invention provides In2Se3The quantum dot application and large-scale stable preparation method has the advantages of small band gap, strong absorption on ultraviolet-visible light wave bands, high carrier mobility and ultrathin property, can reduce the recombination rate of photo-generated electrons and holes, provides a large number of potential reaction active sites with large specific surface area, and improves the photocatalytic performance. In used for the preparation of the invention2Se3The material has good stability and simple preparation, and the photocatalytic efficiency can be obviously improved by introducing air for regulation or using environment to acidity.
Drawings
FIG. 1 shows In prepared In example 12Se3XRD pattern of crystal powder of raw material used for quantum dot.
FIG. 2 shows In prepared In example 12Se3Raman diagram of crystal powder of raw materials used for quantum dots.
FIG. 3 shows In prepared In example 12Se3Quantum dot dispersion liquidThe real object diagram of (1).
FIG. 4 shows In prepared In example 12Se3And (3) carrying out a physical diagram on the quantum dot dispersion liquid under laser irradiation.
FIG. 5 shows In prepared In example 12Se3TEM topography of quantum dots.
FIG. 6 shows In prepared In example 12Se3Particle size statistical chart of quantum dots.
FIG. 7 shows In prepared In example 22Se3TEM topography of quantum dots.
FIG. 8 shows In prepared In example 22Se3Particle size statistical chart of quantum dots.
FIG. 9 shows In prepared In example 22Se3AFM topography of quantum dots.
FIG. 10 shows a portion of In prepared In example 22Se3Height map of quantum dots.
FIG. 11 shows In prepared In example 22Se3Height statistics of quantum dots.
FIG. 12 shows In prepared In example 22Se3Degradation curves of the quantum dots under different conditions.
FIG. 13 shows different In2Se3Degradation curve diagram of the concentration of the dye RhB aqueous solution with the change of illumination time at the beginning of adding amount of the quantum dots.
Detailed Description
The present invention will be described in more detail with reference to the following examples and the accompanying drawings
Example 1
Getting In2Se3Putting 200mg of crystal powder into a wide-mouth bottle, adding 100ml of IPA solvent, performing ultrasonic accumulation for 6 hours at the power of 450W, centrifuging for 20 minutes at 7000rmp/min to obtain quantum dot supernatant, and centrifuging for 30 minutes at the centrifugation rate of 10000rmp/min to precipitate the quantum dots in the solution; washing the precipitate with anhydrous ethanol for 3 times and drying at 40 deg.C to obtain In2Se3And (4) quantum dots.
Due to In2Se3Has a plurality of crystal phases and crystal forms, so that In is prepared2Se3Before quantum dots, it is necessary to determine the crystal phase and crystal form of the raw material crystal powder used. FIG. 1 and FIG. 2 show the preparation of In the present invention2Se3XRD and Raman patterns of the crystal raw material used for the quantum dots; as can be seen from FIG. 1, In was used as a raw material2Se3The crystal powder is matched with the rhombus alpha phase of a laminated structure, has high orientation along the c axis and has good crystallization. The Raman data of FIG. 2 further confirms that alpha phase In is present2Se3。
FIGS. 3 and 4 show In2Se3And (3) a quantum dot dispersion liquid object diagram. As can be seen from FIG. 3, In was prepared2Se3The quantum dot dispersion liquid is transparent and light yellow, and has no obvious small particles and impurities; and no precipitate appears after long-time storage, and the product is stable. FIG. 4 shows In under laser irradiation2Se3The quantum dot dispersion has an obvious Tyndall phenomenon. The resulting mixed system was shown to be homogeneous and a colloid with particle size in the nanometer range dispersed in the supernatant.
FIGS. 5 and 6 show In2Se3TEM morphology and particle size statistic of quantum dots. As can be seen from FIG. 5, after being subjected to ultrasonic treatment for 6h at 450W and centrifugal screening at 7000rmp/min, the quantum dots are relatively uniform In distribution and clear In morphology, the shape of each quantum dot is approximately spherical, the particle sizes of 100 quantum dots In the quantum dots are counted to obtain a graph 6, the particle size distribution is In accordance with normal distribution, most of the particle sizes are between 1.6nm and 3.0nm, the particle sizes account for about 90% of the total number, and In2Se3The average grain diameter of the quantum dots is 2.3 nm.
Example 2
Getting In2Se3Putting 200mg of crystal powder into a wide-mouth bottle, adding 100ml of IPA solvent, performing ultrasonic accumulation for 6 hours at the power of 600W, centrifuging for 20 minutes at 7000rmp/min to obtain quantum dot supernatant, and centrifuging for 30 minutes at the centrifugation rate of 10000rmp/min to precipitate the quantum dots in the solution; washing the precipitate with anhydrous ethanol for 3 times and drying at 40 deg.C to obtain In2Se3And (4) quantum dots.
FIGS. 7 and 8 show In2Se3TEM morphology and particle size statistic of quantum dots. As can be seen from FIG. 7, after being subjected to ultrasonic treatment for 6h at 600W, the quantum dots are relatively uniformly distributed and have clear morphology after being subjected to centrifugal screening at 7000rmp/min, the shape of each quantum dot is approximately spherical, the particle sizes of 100 quantum dots In the quantum dots are counted to obtain a graph 8, the particle size distribution of the quantum dots is known to be In accordance with normal distribution, most of the particle sizes are between 1.4nm and 2.2nm, the particle sizes account for about 85 percent of the total number, and In2Se3The average grain diameter of the quantum dots is 1.8 nm.
FIG. 9, FIG. 10, FIG. 11 are In prepared2Se3AFM topography of quantum dots and their height data. FIG. 10 shows In through which three straight lines In FIG. 9 pass2Se3The quantum dot height diagram shows that the curve has obvious step shape corresponding to the layered structure. FIG. 11 shows 100 In2Se3From the high statistical data obtained for the quantum dots, it can be seen that In2Se3The height of the quantum dots is mostly between 1nm and 3nm, and the average height is about 2 nm. Due to a single layer of In2Se3(Se-In-Se 5 layer atoms) thickness was about 1nm, so that In was prepared2Se3The quantum dots are 2 layers on average.
In obtained In example 22Se3The quantum dots were subjected to the following experiments.
Accurately weighing 4 parts of dye rhodamine B water solution with the concentration of 5ppm by using a measuring cylinder in a 30ml quartz reaction vessel, wherein the dye rhodamine B water solution is numbered as a, B, c and d. Wherein, a is not added with In2Se3The quantum dot photocatalyst is directly placed into a photochemical reactor, a part of solution is taken after magnetic stirring is carried out for 30min under a dark environment, the absorbance within the wavelength range of 400-700nm is tested by an ultraviolet-visible spectrophotometer, and the value at the moment is recorded as 0 min. And pouring the taken part of solution back into the quartz reaction vessel a again, starting a 500W xenon lamp to simulate sunlight irradiation, taking part of solution every 10min to test absorbance, and recording the absorbance for 10min, 20min, 30min, 40min, 50min and 60 min. b adding 5mg of In2Se3Putting the quantum dot photocatalyst into a photochemical reactor, and magnetically stirring for 30min In a dark environment to react In a dark environment to ensure that In is In2Se3The quantum dots are fully contacted with the dye RhB molecules to achieve adsorption-desorption balance. Taking part of the solution after the dark reaction, centrifuging the solution for 5min at 11000rpm/min by using a centrifuge, taking the supernatant, testing the absorbance within the wavelength range of 400-700nm by using an ultraviolet-visible spectrophotometer, and recording the value at the moment as 0 min. And fully oscillating all the taken solutions, pouring the solutions back into the quartz reaction container b again, continuously keeping the magnetic stirring in a dark environment, taking part of the solutions every 10min to test the absorbance, and recording the absorbance for 10min, 20min, 30min, 40min, 50min and 60 min. And c, the experimental step is approximately the same as that of the step b, and the step of changing the step of continuously keeping the magnetic stirring in the dark environment into the step of turning on a 500W xenon lamp to simulate sunlight. And d, in the experiment step, on the basis of c, a 500W xenon lamp is started to simulate the sunlight illumination, and air is introduced at the same time.
FIG. 12 is a graph comparing the degradation effects of four experiments under the above conditions,
in addition, 4 parts of dye rhodamine B water solution with the concentration of 5ppm and the concentration of 20ml are accurately weighed by using a measuring cylinder and are respectively added into a 30ml quartz reaction vessel with the concentration of 3.5mg, 5mg, 7mg and 10mg In2Se3A quantum dot photocatalyst. Placing into a photochemical reaction instrument, magnetically stirring for 30min in dark environment, centrifuging at 11000rpm/min by a centrifuge for 5min, taking the supernatant, testing the absorbance of the supernatant in the wavelength range of 400-700nm by an ultraviolet-visible spectrophotometer, and recording the value as 0 min. Fully oscillating all the taken solutions, pouring the solutions back into respective quartz reaction containers, starting a 500W xenon lamp to simulate sunlight illumination, introducing air, taking part of the solutions every 10min to test absorbance, and recording the absorbance for 10min, 20min, 30min, 40min, 50min and 60 min.
Different In2Se3Degradation curve graph of the concentration of the dye RhB aqueous solution with the change of illumination time at the beginning of adding amount of the quantum dots can be found from FIG. 13, and the degradation curve graph is shown along with In2Se3The initial addition of the quantum dots is increased, the decreasing speed of the RhB aqueous solution concentration is accelerated, and the photocatalytic degradation effect is more obvious.
Claims (9)
1. In2Se3The application of quantum dots is characterized in that,In2Se3application of quantum dots as a photocatalyst in photocatalysis.
2. In2Se3Use of quantum dots, characterized In that2Se3Application of quantum dots as a photocatalyst in photocatalytic degradation of organic dyes.
3. The use according to claim 2, wherein the organic dye is rhodamine B.
4. In2Se3Use of quantum dots, characterized In that2Se3Application of quantum dots in preparation of composite nano-photocatalyst.
5. The use according to any one of claims 1 to 4, wherein In is2Se3The quantum dot size is less than or equal to 5 nm.
6. In2Se3The preparation method of the quantum dot is characterized in that the black phosphorus quantum dot is prepared by adopting the following specific method:
in is mixed with2Se3Adding the crystal powder into a polar solvent, performing ultrasonic treatment for 6h at 600W power in the polar solvent by using a liquid phase stripping method, centrifuging for 20min at 7000rmp/min to obtain a quantum dot supernatant, and centrifuging for 30min at a centrifugation rate of 10000rmp/min to precipitate the quantum dots in the solution; the precipitate was washed 3 times with absolute ethanol and dried at low temperature of 40 ℃ for weighing.
7. In according to claim 62Se3The preparation method of the quantum dot is characterized in that the polar solvent comprises at least one of water, ethanol, isopropanol and N-methyl pyrrolidone.
8. In according to claim 62Se3Preparation method of quantum dotsThe method is characterized in that the ultrasonic power is 450-600W.
9. In according to claim 62Se3The preparation method of the quantum dots is characterized in that the ultrasonic time is 3-12 h, and the centrifugal rate is 7000-10000 rpm.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113332974A (en) * | 2021-06-02 | 2021-09-03 | 广东工业大学 | Modified graphene/tungsten-based nanosheet/magnesium-zinc oxide composite material and preparation method thereof |
CN113332974B (en) * | 2021-06-02 | 2022-08-16 | 广东工业大学 | Modified graphene/tungsten-based nanosheet/magnesium-zinc oxide composite material and preparation method thereof |
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