CN111621297A - Cadmium selenide quantum dot and solid-phase preparation method thereof - Google Patents
Cadmium selenide quantum dot and solid-phase preparation method thereof Download PDFInfo
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Abstract
The invention provides a cadmium selenide quantum dot and a solid phase preparation method thereof, wherein the solid phase preparation method comprises the following steps: uniformly mixing a cation precursor and an anion precursor at room temperature to form a mixture A; adding inorganic substance powder into the mixture A, and grinding and uniformly mixing to obtain a mixture B; and placing the mixture B in a crucible, and calcining in a muffle furnace to obtain the cadmium selenide quantum dots. According to the invention, the cadmium selenide quantum dots are prepared by calcining the anion/cation precursor at high temperature, only a small amount of organic solvent is needed to dissolve the cation precursor, and in the high-temperature calcination process, the small amount of organic solvent is completely volatilized, and the quantum dots can be directly used by dispersing in inorganic powder without using the organic solvent for multiple precipitation and purification, so that the method has better environmental friendliness.
Description
Technical Field
The invention relates to the technical field of luminescent materials, in particular to a cadmium selenide quantum dot and a solid-phase preparation method thereof.
Background
The quantum dots as a new generation luminescent material have the outstanding characteristics of narrow half-peak width, adjustable color, luminous efficiency and the like, and have wide application prospects in the field of photoelectric devices such as light-emitting diodes, light sources, displays, solar cells, fluorescent labels and the like. Among various quantum dots, cadmium selenide quantum dots have wide adjustable range of emission wavelength from infrared spectrum to ultraviolet spectrum; the repairability is strong, and various later-period coating and modification are convenient to carry out; and the stability is good, so the method has wide application in various fields.
However, the existing cadmium selenide quantum dots are generally prepared in an organic phase by a high-temperature thermal injection method, and a great amount of organic solvent is needed in the later-stage quantum dot purification, which results in the generation of a great amount of organic waste liquid. Therefore, the liquid phase synthesis method not only keeps the preparation cost of the quantum dots high, but also cannot realize batch production; on the other hand, a large amount of organic waste liquid generated in the preparation process also causes great harm to the environment.
Disclosure of Invention
The invention solves the problems that: how to provide an environment-friendly method for preparing cadmium selenide quantum dots.
In order to solve the problems, the invention provides a solid-phase preparation method of cadmium selenide quantum dots, which comprises the following steps:
uniformly mixing a cation precursor and an anion precursor at room temperature to form a mixture A; adding inorganic substance powder into the mixture A, and grinding and uniformly mixing to obtain a mixture B; and placing the mixture B in a crucible, and calcining in a muffle furnace to obtain the cadmium selenide quantum dots.
Optionally, the mass ratio of the cationic precursor to the anionic precursor is (1-8): (1-2).
Optionally, the cation precursor comprises one or more of cadmium oleate, cadmium stearate, cadmium laurate, cadmium chloride, cadmium nitrate, cadmium sulfate, cadmium oxalate and cadmium acetate; the anion precursor comprises one or more of selenium powder, trioctyl selenium phosphine, selenol, diselenide, selenide, selenoate and selenamide.
Optionally, the inorganic powder has a particle size of 50nm to 5 μm.
Optionally, the mass ratio of the inorganic powder to the mixture A is (1-2): (5-10).
Optionally, the inorganic substance powder includes one or more of silicon powder, molecular sieve powder, alumina powder, calcium carbonate powder, barium sulfate powder, montmorillonite powder and montmorillonite modifier powder.
Optionally, the conditions for performing calcination in the muffle furnace include: the temperature is 200 ℃ and 350 ℃, and the calcination time is 5-30 min.
Optionally, the method further comprises: and carrying out ball milling on the cadmium selenide quantum dots.
Optionally, the ball milling conditions include: the ball milling speed is 50-100r/min, and the ball milling time is 5 min.
Compared with the prior art, the solid-phase preparation method of the cadmium selenide quantum dots provided by the invention has the following advantages:
(1) according to the invention, the cadmium selenide quantum dots are prepared by calcining the anion/cation precursor at high temperature, on one hand, in the preparation step of the quantum dots, only a small amount of organic solvent is needed to dissolve the cation precursor, and in the high-temperature calcination process, the small amount of organic solvent is completely volatilized; on the other hand, by dispersing the quantum dots in the inorganic powder, the quantum dots can be used without performing multiple precipitation purifications using an organic solvent.
(2) The solid phase preparation method provided by the invention has the advantages of simple process and mild conditions, effectively reduces the use of organic solvents, reduces the production cost, and can realize the controllable emission wavelength of the cadmium selenide quantum dots by regulating and controlling the calcination time and adding different inorganic substances, thereby expanding the commercial value of the cadmium selenide quantum dots.
The invention also aims to provide the cadmium selenide quantum dot to solve the problem that the existing cadmium selenide quantum dot uses a large amount of organic solvent in the preparation process.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the cadmium selenide quantum dot is prepared according to the solid-phase preparation method of the cadmium selenide quantum dot.
Compared with the prior art, the solid-phase preparation method of the cadmium selenide quantum dot has the same advantages as the solid-phase preparation method of the cadmium selenide quantum dot, and is not described herein again.
Drawings
Fig. 1 is a schematic flow chart of a solid-phase preparation method of cadmium selenide quantum dots according to the present invention;
FIG. 2 is a scanning electron microscope image of a cadmium selenide quantum dot in accordance with the present invention;
FIG. 3 is a fluorescence emission spectrum of a cadmium selenide quantum dot according to example 1 of the present invention;
FIG. 4 is a fluorescence emission spectrum of a cadmium selenide quantum dot according to example 2 of the present invention;
fig. 5 is a fluorescence emission spectrum of the cadmium selenide quantum dot according to embodiment 3 of the invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
In addition, the terms "comprising," "including," "containing," and "having" are intended to be non-limiting, i.e., that other steps and other ingredients can be added that do not affect the results. Materials, equipment and reagents are commercially available unless otherwise specified.
In addition, although the invention has described the forms of S1, S2, S3 and the like for each step in the preparation, the description is only for the convenience of understanding, and the forms of S1, S2, S3 and the like do not represent the limitation of the sequence of each step.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
With reference to fig. 1, the present invention provides a solid phase preparation method of cadmium selenide quantum dots, comprising the steps of:
s1, uniformly mixing the cation precursor and the anion precursor at room temperature to form a mixture A;
s2, adding inorganic matter powder into the mixture A, and grinding and uniformly mixing to obtain a mixture B;
and S3, placing the mixture B in a crucible, and calcining in a muffle furnace to obtain the cadmium selenide quantum dot.
It can be understood that the traditional synthesis of the cadmium selenide quantum dot is generally divided into two steps of synthesis and purification, and in the synthesis step, in order to improve the reaction stability of an anion/cation precursor, the synthesis needs to be carried out in a large amount of high-boiling-point organic solvent; the quantum dots prepared by the method are dispersed in an organic solvent at a relatively dilute concentration (the solid content is usually less than 5%), a large amount of poor solvent is usually required to be added, the quantum dots are precipitated from the reaction system, and the steps generate a large amount of organic waste liquid.
Compared with the traditional liquid phase synthesis method, the preparation method of the cadmium selenide quantum dot provided by the invention prepares the cadmium selenide quantum dot by calcining the anion/cation precursor at high temperature, on one hand, in the preparation step of the quantum dot, only a small amount of organic solvent is needed to dissolve the cation precursor, and in the high-temperature calcination process, the small amount of organic solvent is completely volatilized; on the other hand, by dispersing the quantum dots in the inorganic powder, the inorganic powder can serve as a carrier and help the dispersion of the quantum dots, and thus can be used without precipitation using a large amount of a poor solvent. The solid-phase preparation method provided by the invention has the advantages of simple process, simplified preparation steps, avoidance of massive use of organic solvents in a liquid-phase synthesis method, environmental friendliness, low cost and contribution to large-scale preparation.
In step S1, the cation precursor includes one or more of cadmium oleate, cadmium stearate, cadmium laurate, cadmium chloride, cadmium nitrate, cadmium sulfate, cadmium oxalate, and cadmium acetate.
Wherein, the cation precursor can be prepared by a conventional method, and can also be directly purchased and used as a finished product. In the embodiment of the invention, when the cationic precursor is cadmium oleate, the preparation method specifically comprises the following steps:
the cadmium precursor is prepared from cadmium oxide, oleic acid and octadecylene, for example, cadmium salt, oleic acid and octadecylene are mixed, and then the cadmium precursor solution is obtained by vacuumizing, heating to more than 100 ℃, vacuumizing again and heating again to 220-240 ℃ until the mixed solution is clear and transparent, wherein the concentration of the cadmium precursor can be 0.2-0.6 mol/L.
The anion precursor comprises one or more of selenium powder, trioctyl selenium phosphine, selenol, diselenide, selenide, selenoate and selenamide. In the embodiment of the present invention, the anionic precursor is preferably selenium powder.
In order to ensure sufficient reaction, in the embodiment of the present invention, the mass ratio of the cationic precursor to the anionic precursor is (1-8): (1-2), and preferably, the mass ratio of the cationic precursor to the anionic precursor is (1-4): 1.
In step S2, in the embodiment of the present invention, inorganic powder is used as a carrier of the quantum dot, and the cationic precursor and the anionic precursor are attached to the surface of the inorganic powder, so as to disperse and dilute the raw material and ensure the particle size distribution of the synthesized quantum dot, wherein the particle size of the inorganic powder is 50nm to 5 μm.
Specifically, the inorganic powder and the mixture A are mixed according to the mass ratio of (1-2) to (5-10), and are ground and stirred uniformly to form a mixture B.
Wherein the inorganic substance powder comprises one or more of silicon powder, molecular sieve powder, aluminum oxide powder, calcium carbonate powder, barium sulfate powder, montmorillonite powder and montmorillonite modified substance powder.
In step S3, specifically, the mixture B of the cation precursor and the anion precursor attached to the surface of the inorganic powder is placed in a crucible, and is placed in a muffle furnace, and is calcined at 350 ℃ for 5-30min, and then the crucible is removed and cooled to room temperature, so as to generate the cadmium selenide quantum dots with the inorganic substance as the matrix, that is, the quantum dots are dispersed in the inorganic oxide matrix.
Inorganic powder is used as a carrier for generating the quantum dots by the reaction of a cation precursor and an anion precursor, so that the agglomeration phenomenon in the crystallization process of the quantum dots can be effectively inhibited in the calcining process, and meanwhile, the size distribution of the quantum dots can be well controlled; in addition, the pore size distribution of the inorganic powder can be controlled by adjusting the calcination time, so that the emission wavelength of the quantum dots can be effectively regulated, the quantum dot materials with different fluorescence colors can be obtained, and the application value of the cadmium selenide quantum dots is expanded.
Further, the solid-phase preparation method of the cadmium selenide quantum dot using the inorganic substance as the matrix provided by the embodiment of the invention further comprises the following steps:
s4, performing ball milling on the cadmium selenide quantum dots prepared in the step S3. Wherein, the ball milling conditions comprise: the ball milling speed is 50-100r/min, and the ball milling time is 5 minutes.
After high-temperature calcination, inorganic substance powder may be agglomerated, so the obtained cadmium selenide quantum dot powder particle using the inorganic substance as a matrix is large, and in practical application, the large particle is not easy to disperse in a plastic or glue matrix, which is easy to cause product defects. Therefore, the particle size of the cadmium selenide quantum dot powder can be further reduced by ball-milling the prepared cadmium selenide quantum dot again so as to meet the requirements of practical application.
The invention also provides a cadmium selenide quantum dot, which is prepared by the solid-phase preparation method of the cadmium selenide quantum dot, wherein in the prepared cadmium selenide quantum dot, the quantum dot is dispersed in an inorganic oxide matrix.
Fig. 2 is an electron microscope image of cadmium selenide quantum dots, and it can be seen from fig. 2 that inorganic substance powder is used as a carrier of the quantum dots, and the quantum dots are attached to the surface of the inorganic oxide, so that the particle size distribution of the synthesized cadmium selenide quantum dots is ensured.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are examples of experimental procedures not specified under specific conditions, generally according to the conditions recommended by the manufacturer.
Example 1
The embodiment provides a solid-phase preparation method of cadmium selenide quantum dots, which comprises the following specific steps:
s1, placing 1.28 g of 10mmol of cadmium oxide, 10mL of oleic acid and 10mL of octadecene in a three-neck flask, heating to 120 ℃, and pumping gas for 3 times at intervals of 10min by a vacuum oil pump and a balloon filled with high-purity argon to remove water and oxygen in the reaction system; and then under the protection of inert gas, uniformly stirring the reactants, and gradually heating to 230 ℃ until the system becomes a clear solution, thus obtaining the 0.5M cadmium oleate precursor.
Weighing 1mmol of selenium powder, adding 4mL of prepared 0.5M cadmium oleate precursor, namely, the mass ratio of the cation precursor to the anion precursor is 2: 1, stirring and mixing uniformly to form a mixture A;
s2, adding 1.5 g of MCM-41 molecular sieve powder into the mixture A, namely, the mass ratio of the inorganic substance powder to the mixture A is 1: 1, further grinding and uniformly mixing to obtain a mixture B;
and S3, transferring the mixture B into a crucible in an air atmosphere, calcining the mixture B in a muffle furnace at 250 ℃ for 5 minutes, taking out the crucible after the reaction is finished, and cooling the crucible to room temperature to obtain the cadmium selenide quantum dots taking the molecular sieve powder as the matrix.
With reference to fig. 3, the prepared cadmium selenide quantum dots using the molecular sieve powder as the matrix were analyzed by fluorescence spectroscopy, and the fluorescence emission wavelength was 576 nm.
Example 2
This example differs from example 1 in that:
in the step S3, transferring the mixture B into a crucible in the air atmosphere, calcining the mixture B in a muffle furnace at 250 ℃ for 7 minutes, taking out the crucible after the reaction is finished, and cooling the crucible to room temperature to obtain the cadmium selenide quantum dots taking the molecular sieve powder as the matrix;
the other steps are the same as in parametric example 1.
With reference to fig. 4, the prepared cadmium selenide quantum dots using the molecular sieve powder as the matrix were analyzed by fluorescence spectroscopy, and the fluorescence emission wavelength was 585 nm.
Example 3
The difference between the embodiment and embodiment 1 is that a solid-phase preparation method of cadmium selenide quantum dots is provided, which specifically includes the following steps:
s1, under the protection of inert gas, 3.14 g of 5mmol of cadmium stearate and 5mL of octadecene are placed in a flask, and the flask is heated at 200 ℃ until the cadmium stearate is completely dissolved, so that 0.5M cadmium stearate precursor is obtained.
Weighing 0.5mmol selenium powder, adding 2mL of prepared 0.5M cadmium stearate precursor, namely the mass ratio of the cation precursor to the anion precursor is 2: 1 stirring and mixing uniformly to form a mixture A;
s2, adding 0.75 g of 4A molecular sieve powder to the mixture a, that is, the mass ratio of the inorganic powder to the mixture a is 1: 1, further grinding and uniformly mixing to obtain a mixture B;
and S3, transferring the mixture B into a crucible in an air atmosphere, calcining the mixture B in a muffle furnace at 250 ℃ for 7 minutes, taking out the crucible after the reaction is finished, and cooling the crucible to room temperature to obtain the cadmium selenide quantum dots taking the molecular sieve powder as the matrix.
With reference to fig. 5, the prepared cadmium selenide quantum dots using the molecular sieve powder as the matrix were analyzed by fluorescence spectroscopy, and the fluorescence emission wavelength was 580 nm.
The preparation method disclosed by the invention is simple in process and mild in condition, effectively reduces the use of organic solvents, reduces the production cost, and can realize the controllable emission wavelength of the cadmium selenide quantum dots by regulating and controlling the calcination time and adding different inorganic substances, thereby expanding the commercial value of the cadmium selenide quantum dots.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.
Claims (10)
1. A solid-phase preparation method of cadmium selenide quantum dots is characterized by comprising the following steps:
uniformly mixing a cation precursor and an anion precursor at room temperature to form a mixture A;
adding inorganic substance powder into the mixture A, and grinding and uniformly mixing to obtain a mixture B;
and placing the mixture B in a crucible, and calcining in a muffle furnace to obtain the cadmium selenide quantum dots.
2. The solid phase preparation method of cadmium selenide quantum dots according to claim 1, wherein the mass ratio of the cation precursor to the anion precursor is (1-8) to (1-2).
3. The solid-phase preparation method of the cadmium selenide quantum dot according to claim 2, wherein the cation precursor comprises one or more of cadmium oleate, cadmium stearate, cadmium laurate, cadmium chloride, cadmium nitrate, cadmium sulfate, cadmium oxalate and cadmium acetate; the anion precursor comprises one or more of selenium powder, trioctyl selenium phosphine, selenol, diselenide, selenide, selenoate and selenamide.
4. The solid-phase preparation method of the cadmium selenide quantum dot according to claim 1, wherein the particle size of the inorganic substance powder is 50nm to 5 μm.
5. The solid-phase preparation method of cadmium selenide quantum dots according to claim 4, wherein the mass ratio of the inorganic substance powder to the mixture A is (1-2) to (5-10).
6. The solid-phase preparation method of the cadmium selenide quantum dot according to claim 5, wherein the inorganic substance powder comprises one or more of silicon powder, molecular sieve powder, aluminum oxide powder, calcium carbonate powder, barium sulfate powder, montmorillonite powder and montmorillonite modifier powder.
7. The solid-phase preparation method of the cadmium selenide quantum dot according to claim 1, wherein the calcining in a muffle furnace is performed under the conditions comprising: the calcination temperature is 200-350 ℃, and the calcination time is 5-30 min.
8. The solid-phase preparation method of the cadmium selenide quantum dot according to claim 1, further comprising: and carrying out ball milling on the cadmium selenide quantum dots.
9. The solid-phase preparation method of the cadmium selenide quantum dot according to claim 8, wherein the ball milling conditions comprise: the ball milling speed is 50-100r/min, and the ball milling time is 5 min.
10. A cadmium selenide quantum dot, which is prepared by the solid-phase preparation method of the cadmium selenide quantum dot according to any one of claims 1 to 9.
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