CN110776908A - Method for preparing zinc oxide quantum dots in ultrasonic-assisted manner by incomplete solute dissolution - Google Patents
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Abstract
The invention discloses a method for preparing zinc oxide quantum dots by ultrasonic assistance in a solute incomplete dissolving mode. The technical scheme comprises the following preparation method: step 1: putting zinc-containing inorganic salt into an alcohol organic solvent in an ultrasonic environment to form ZnO precursor suspension A; step 2: fully dissolving strong base in an alcohol organic solvent in a stirring environment to obtain a clear solution B; and step 3: dropwise adding the clear solution B obtained in the step 2 into the suspension A obtained in the step 1 in an ultrasonic environment, and allowing the clear solution B to fully react in the ultrasonic environment for 10-40min to obtain a solution C; and 4, step 4: adding the solution C reacted in the step 3 into a nonpolar solvent, standing for precipitation, centrifuging at a certain speed, removing a supernatant to obtain an initial precipitate, then adding an alcohol organic solvent, and dispersing the precipitate in an ultrasonic environment; and 5: repeating the step 4 for more than two times to obtain pure ZnO quantum dot precipitate; step 6: and (5) placing the ZnO quantum dot precipitate obtained in the step (5) in a vacuum drier for annealing treatment to obtain ZnO powder.
Description
Technical Field
The invention belongs to the field of semiconductor nano materials, and particularly relates to a method for preparing zinc oxide quantum dots.
Background
Quantum dots (quantum dots) refer to a functional nanomaterial with semiconductor particle size small enough to be between 1-20nm in three-dimensional scale. Quantum dots are generally spherical or spheroidal and are typically composed of group IV, II-VI, or III-V elements. The size effect of quantum dots results in their generally optoelectronic properties that are not possessed by macroscopic bulk materials, which emit light of a specific wavelength or frequency by applying a certain optical pressure or electric field to the quantum dots. Common quantum dot materials include cadmium sulfide quantum dots, cadmium selenide quantum dots, cadmium telluride quantum dots, lead sulfide quantum dots, and the like. Compared with the common quantum dots, the zinc oxide (ZnO) quantum dots have the advantages of no toxicity, no harm, environmental friendliness and the like. Meanwhile, the zinc oxide has a wider forbidden band width (3.2 eV) and stronger exciton binding energy (60 meV), and is a semiconductor material with important application value. It is currently used in many applications, such as photocatalysis, sensors, solar cells, biomedicine, ceramic materials, rubber industry, etc.
The existing method for preparing the zinc oxide quantum dots mainly comprises a sol-gel method and a hydrothermal synthesis method. The specific treatment means of the method comprises high-temperature treatment, reflux high-power stirring and the like, and the energy consumption and the cost are high. Meanwhile, in the existing preparation methods of ZnO quantum dots, the fact that the preparation of a precursor part particularly emphasizes that the quantum dots can be prepared only after a solute is required to be completely dissolved and a completely transparent and clear solution is prepared is particularly emphasized. This results in a long time of the required preparation process, limiting its popularization and application, and also hampering the research on the nucleation mechanism in the field of quantum dots.
Disclosure of Invention
The invention aims to provide a method for preparing zinc oxide quantum dots in an ultrasonic-assisted manner by incomplete dissolution of a solute.
In order to solve the problems, the technical scheme adopted by the invention comprises the following preparation method:
step 1: putting zinc-containing inorganic salt into an alcohol organic solvent in an ultrasonic environment to form ZnO precursor suspension A;
step 2: fully dissolving strong base in an alcohol organic solvent in a stirring environment to obtain a clear solution B;
and step 3: dropwise adding the clear solution B obtained in the step 2 into the suspension A obtained in the step 1 in an ultrasonic environment, and allowing the clear solution B to fully react in the ultrasonic environment for 10-40min to obtain a solution C;
and 4, step 4: adding the solution C reacted in the step 3 into a nonpolar solvent, standing for precipitation, centrifuging at a certain speed, removing a supernatant to obtain an initial precipitate, then adding an alcohol organic solvent, and dispersing the precipitate in an ultrasonic environment;
and 5: repeating the step 4 for more than two times to obtain pure ZnO quantum dot precipitate;
step 6: and (5) placing the ZnO quantum dot precipitate obtained in the step (5) in a vacuum drier for annealing treatment to obtain ZnO powder.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in the steps 1 and 3, the ultrasonic power of the ultrasonic wave is 200-.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in the steps 1 and 2, the alcohol organic solvent is absolute ethyl alcohol, and the purity of the alcohol organic solvent is chromatographic purity.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in the step 1, the concentration of zinc salt in the suspension A is 0.01-0.4mol/L, and the adopted zinc-containing inorganic salt is zinc acetate dihydrate.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in step 2, the strong base is lithium hydroxide monohydrate, and the molar solution concentration of the lithium hydroxide monohydrate in the solution is 0.2-0.5 mol/L.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in step 1, the amount ratio of the zinc salt of the zinc-containing inorganic salt to the alkali is 1: 0.2-1: 1.
the method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in step 3, the clear solution B obtained in step 2 is added dropwise into the suspension A obtained in step 1 through a constant-pressure separating funnel to obtain a solution C.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in step 4, the non-polar organic solvent is: one of n-heptane, n-hexane, toluene, dichloromethane and chloroform, wherein the volume ratio of the used alcohol organic solvent to the nonpolar solvent is 1: 2-1: 4.
the method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in step 4, the centrifugation speed is 2000-6000r/min, and the centrifugation time is 10-20 min.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in step 6, the annealing temperature is 50-100 ℃, and the used equipment is a vacuum drying oven.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: the ultrasonic environment is composed of an ultrasonic generating device with a water circulation constant temperature system.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode is characterized by comprising the following steps: in step 1, step 2, and step 3, the mixing is performed in a mixed environment composed of an ultrasonic environment and a stirring environment.
The method for preparing the zinc oxide quantum dots by the ultrasonic assistance in the incomplete solute dissolving mode has the following advantages:
1. this patent relies on 2016 national key research and development project-international scientific and technological innovation cooperation key special item between government of the department of science and technology (middle and American): the project of 'control strategy and method research for improving the uniformity of nano-component film' is supported, and the project number is as follows: 2016YFE 0105900. Compared with the traditional chemical method, the synthesis speed of the zinc oxide quantum dots can be increased by the aid of ultrasonic auxiliary treatment, the operation is simple and convenient, and the cost is low. The prepared quantum dot has high luminous intensity and quantum dot yield.
2. The method has the advantages of safety, no toxicity, environmental friendliness, good particle uniformity, high quantum yield, good luminescence property and the like.
Drawings
FIG. 1 is a TEM image of zinc oxide quantum dots prepared by the method of the present invention;
FIG. 2 is an HRTEM image of zinc oxide quantum dots prepared by the method of the present invention;
FIG. 3 is an XRD pattern of zinc oxide quantum dots prepared by the method of the present invention;
FIG. 4 is an electron diffraction pattern of zinc oxide quantum dots prepared by the method of the present invention;
FIG. 5 is a graph showing the luminescence of zinc oxide quanta prepared by the method of the present invention.
Detailed Description
Referring to fig. 1-5, the method for preparing zinc oxide quantum dots by ultrasonic assistance in the incomplete solute dissolving mode comprises the following specific steps:
step 1: 1.6g of zinc acetate dihydrate is weighed, added into 50mL of absolute ethanol (the purity is chromatographic purity), and mixed for 20min in an ultrasonic environment to form a ZnO precursor suspension A. During the period, the ultrasonic power of the ultrasonic wave generating device is controlled to be 300W, the ultrasonic temperature is controlled to be 40 ℃, so that the zinc acetate dihydrate and the absolute ethyl alcohol are fully mixed.
Step 2: 0.38g of lithium hydroxide monohydrate was weighed and added to 25mL of absolute ethanol (the purity was chromatographically pure) and stirred at room temperature for 30min to form a colorless transparent alkaline solution, and a clear solution B was obtained.
And step 3: and (3) in an ultrasonic environment, dropwise adding the clear solution B obtained in the step (2) into the suspension A obtained in the step (1), and allowing the clear solution B to fully react in the ultrasonic environment for 20min to obtain a solution C. And in the period, the ultrasonic power of the ultrasonic wave generating device is controlled to be 300W, and the ultrasonic temperature is controlled to be 40 ℃, so that the clear solution B and the suspension A are fully reacted.
And 4, step 4: according to the following steps of 1: 2, adding the solution C after the reaction in the step 3 into a non-polar solvent, and standing and precipitating for 20 minutes. After the precipitate was completely precipitated, the liquid was centrifuged at 4000r/min and the supernatant was removed to obtain the initial precipitate. Then 10mL of absolute ethanol solution is added, and the mixture is dispersed in absolute ethanol again by ultrasonic treatment for 2min to form colorless transparent liquid.
And 5: repeating the process of the step 4 for 3 times to obtain pure ZnO quantum dot precipitate, and recording the precipitate as liquid D.
Step 6: and (5) placing the ZnO quantum dot precipitate obtained in the step (5) in a vacuum drier for annealing treatment to obtain ZnO powder. The annealing temperature is 50-100 ℃, and the used equipment is a vacuum drying oven.
The zinc oxide quantum dot with the particle size of 1-10nm, the fluorescence range of 370-690nm and the quantum yield of more than 50 percent can be obtained by adopting the preparation method.
Preferably, in step 1, the concentration of the zinc acetate dihydrate is 0.01-0.4mol/L, so as to obtain the optimal concentration under the condition of proper amplification.
Preferably, in step 2, the strong base is lithium hydroxide monohydrate having a molar solution concentration of 0.2 to 0.5mol/L in solution, to achieve suitable scale-up in the case of obtaining an optimum concentration.
Preferably, in step 1, the amount ratio of the zinc salt of the zinc-containing inorganic salt to the alkali is 1: 0.2-1: 1, to be properly enlarged in case of obtaining an optimal ratio.
Preferably, in the step 3, the clear solution B obtained in the step 2 is dropwise added into the suspension A obtained in the step 1 through a constant-pressure separating funnel to obtain a solution C, and the dropwise addition is performed to ensure the uniformity of the product and ensure the nucleation and growth processes in the quantum dot reaction process, so that the reaction product is more uniform.
Preferably, in step 4, the non-polar organic solvent is: one of n-heptane, n-hexane, toluene, dichloromethane and chloroform. The surface of the quantum dot prepared by the reaction is not modified with a ligand, so that a product can be obtained by changing a solution polar system. Compared with the method of adding a long-chain ligand (such as oleic acid) in the synthesis process, the method is simpler and more convenient to operate, and meanwhile, the modification of the ligand usually causes the change of a surface group of the quantum dot, so that the subsequent operation is not facilitated.
Preferably, the ultrasonic environment is formed by an ultrasonic generating device with a water circulation constant temperature system. Compared with the traditional magnetic and mechanical stirring mode, the ultrasonic wave has remarkable advantages. The frequency of the ultrasonic waves is very high, so that the products can be more fully mixed uniformly, and the experimental result is ensured. However, due to the limitation of the ultrasonic generator device, the temperature and the change of the reaction cannot be accurately controlled, so that the temperature control mode with water circulation is adopted, and the ultrasonic generator can prepare temperature control and heat preservation.
Preferably, in step 1, step 2 and step 3, the mixing environment consisting of an ultrasonic environment and a stirring environment is respectively performed, so that the solution is fully dissolved and reacted.
The beneficial effects of the invention are further illustrated by the following test examples: the result of the test using the XRD equipment after drying by dropping the solution D on the XRD sample stage is shown in FIG. 3. Each diffraction peak corresponds to ZnO standard card 36-1451 respectively, and it can be seen that the sample peak has no large peak shift, which indicates that the ZnO precursor has been completely converted into ZnO quantum dots, and each diffraction peak of XRD is strong and the peak type is sharp. This indicates that the crystallinity of this sample is good.
The liquid D is dripped on a carbon net supporting net, and a result of a test by a transmission electron microscope after drying is shown in figure 1, wherein the particles have no obvious agglomeration and aggregation, the particle appearance is consistent (spherical), and the distribution is uniform. According to the HRTEM result, the prepared sample can be seen (figure 2) to have clear lattice fringes, which shows that the crystallization condition is good, and the average value of the particle sizes of the prepared sample is 4nm through statistics. According to the electron diffraction pattern (fig. 4), the prepared ZnO quantum dots have a hexagonal wurtzite structure, and no other polycrystalline or amorphous structure exists.
In the scheme, the volume ratio of the used alcohol organic solvent to the nonpolar solvent is 1: 2-1: 4 range; in the steps 1 and 3, the ultrasonic power of the ultrasonic wave is 200-; in step 4, the centrifugation speed is 2000-6000r/min, and the centrifugation time is within the range of 10-20 min. The effects of the present invention can be achieved.
Although the present invention has been described with reference to the above embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A method for preparing zinc oxide quantum dots by ultrasonic assistance in a solute incomplete dissolution mode is characterized in that the particle size range of the zinc oxide quantum dots is 1-10nm, the fluorescence range is 370-690nm, and the quantum yield is more than 50%, and the method comprises the following steps:
step 1: putting zinc-containing inorganic salt into an alcohol organic solvent in an ultrasonic environment to form ZnO precursor suspension A;
step 2: fully dissolving strong base in an alcohol organic solvent in a stirring environment to obtain a clear solution B;
and step 3: dropwise adding the clear solution B obtained in the step 2 into the suspension A obtained in the step 1 in an ultrasonic environment, and allowing the clear solution B to fully react in the ultrasonic environment for 10-40min to obtain a solution C;
and 4, step 4: adding the solution C reacted in the step 3 into a nonpolar solvent, standing for precipitation, centrifuging at a certain speed, removing a supernatant to obtain an initial precipitate, then adding an alcohol organic solvent, and dispersing the precipitate in an ultrasonic environment;
and 5: repeating the step 4 for more than two times to obtain pure ZnO quantum dot precipitate;
step 6: and (5) placing the ZnO quantum dot precipitate obtained in the step (5) in a vacuum drier for annealing treatment to obtain ZnO powder.
2. The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode according to claim 1, wherein the method comprises the following steps: in the steps 1 and 3, the ultrasonic power of the ultrasonic wave is 200-.
3. The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode according to claim 1, wherein the method comprises the following steps: in the steps 1 and 2, the alcohol organic solvent is absolute ethyl alcohol, and the purity of the alcohol organic solvent is chromatographic purity.
4. The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode according to claim 1, wherein the method comprises the following steps: in the step 1, the concentration of the zinc-containing inorganic salt in the suspension A is 0.01-0.4mol/L, and the adopted zinc-containing inorganic salt is zinc acetate dihydrate.
5. The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode according to claim 1, wherein the method comprises the following steps: in step 2, the strong base is lithium hydroxide monohydrate, and the molar solution concentration of the lithium hydroxide monohydrate in the solution is 0.2-0.5 mol/L.
6. The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode according to claim 1, wherein the method comprises the following steps: in step 1, the amount ratio of the zinc salt of the zinc-containing inorganic salt to the alkali is 1: 0.2-1: 1.
7. the method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode according to claim 1, wherein the method comprises the following steps: in step 3, the clear solution B obtained in step 2 is added dropwise into the suspension A obtained in step 1 through a constant-pressure separating funnel to obtain a solution C.
8. The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode according to claim 1, wherein the method comprises the following steps: in step 4, the non-polar organic solvent is: one of n-heptane, n-hexane, toluene, dichloromethane and chloroform, wherein the volume ratio of the used alcohol organic solvent to the nonpolar solvent is 1: 2-1: 4.
9. the method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode according to claim 1, wherein the method comprises the following steps: in step 4, the centrifugation speed is 2000-6000r/min, and the centrifugation time is 10-20 min.
10. The method for preparing the zinc oxide quantum dots by the ultrasonic assistance of the incomplete solute dissolving mode according to claim 1, which is characterized in that: in step 6, the annealing temperature is 50-100 ℃, and the used equipment is a vacuum drying oven.
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| WO2021082960A1 (en) * | 2019-10-31 | 2021-05-06 | 温州大学激光与光电智能制造研究院 | Method for preparing zinc oxide quantum dots by ultrasonic wave assistance in solute incomplete dissolution mode |
| WO2022143435A1 (en) * | 2020-12-30 | 2022-07-07 | Tcl科技集团股份有限公司 | Quantum dot screening method and quantum dot light-emitting diode |
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| CN108611088A (en) * | 2018-05-22 | 2018-10-02 | 温州大学苍南研究院 | A kind of method that sonochemical method prepares ZnO quantum dot |
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| CN110776908A (en) * | 2019-10-31 | 2020-02-11 | 温州大学激光与光电智能制造研究院 | Method for preparing zinc oxide quantum dots in ultrasonic-assisted manner by incomplete solute dissolution |
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| ERIC A. MEULENKAMP: "Synthesis and Growth of ZnO Nanoparticles", 《J. PHYS. CHEM. B》 * |
| WEIMIN YANG ET AL.: "ast synthesize ZnO quantum dots via ultrasonic method", 《ULTRASONICS SONOCHEMISTRY》 * |
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| WO2021082960A1 (en) * | 2019-10-31 | 2021-05-06 | 温州大学激光与光电智能制造研究院 | Method for preparing zinc oxide quantum dots by ultrasonic wave assistance in solute incomplete dissolution mode |
| WO2022143435A1 (en) * | 2020-12-30 | 2022-07-07 | Tcl科技集团股份有限公司 | Quantum dot screening method and quantum dot light-emitting diode |
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