CN112742687B - Controllable preparation method of orderly-arranged lead sulfide quantum dots - Google Patents
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Abstract
The invention provides a controllable preparation method of orderly-arranged lead sulfide quantum dots, and belongs to the technical field of quantum dot preparation. The preparation method innovatively adopts a two-dimensional planar material with a grid structure as a template, and the controllable growth and ordered distribution of the lead sulfide quantum dots are realized by dispersing the lead sulfide sol on the two-dimensional material. The whole preparation method is simple and easy to realize, and the quantum dots with uniform particle size distribution and special arrangement can be finally prepared.
Description
Technical Field
The invention belongs to the technical field of quantum dot preparation, and particularly relates to a controllable preparation method of orderly-arranged lead sulfide quantum dots.
Background
The quantum dots are also called nano crystals, the size of three dimensions of the quantum dots is less than 100nm, the quantum dots are composed of a small number of atoms, and therefore the quantum dots are similar to a dot in shape and are an emerging low-dimensional photoelectric material. The carrier is confined in a three-dimensional space and cannot move freely due to size limitation, so that the carrier has obvious quantum confinement effect, and the absorption spectrum can be adjusted by controlling the particle size. Since 1993, after the research on the synthesis of CdX (X ═ S, Se, Te) quantum dots by the american Bawendi group of science and technology in the state of ma through an organometallic method, the research activities on quantum dots have been vigorously developed, and the preparation process and the photoelectric characteristics thereof have been widely researched and also successfully applied to various fields such as detection imaging, illumination, biomedical, solar cells, and the like.
Among the quantum dots, the IV-VI family quantum dots are widely concerned because of the large bohr radius of the exciton and the small band gap. The lead sulfide quantum dots are distinguished from many quantum dots due to the advantages of exciton Bohr radius of up to 18nm, symmetrical energy band structure, larger dielectric constant, good photoelectric characteristic, continuously adjustable band gap and the like, and are widely applied to the fields of photoelectric detection, light-emitting diodes, solar cells, biological tracing and the like.
The traditional preparation method of the lead sulfide quantum dots is divided into two main categories: physical methods and chemical methods. The common method for synthesizing high-quality colloidal lead sulfide quantum dots in recent years mainly comprises a colloid chemical method, a vapor deposition method, a microemulsion method, an electrochemical deposition method, a template method, a hydrothermal method and the like, and the synthesized quantum dots are separated and purified and then stored in an organic solvent for subsequent operation. In view of the development of the future technology of quantum dots prepared by using a solution process, how to assemble an integrated structure and realize ordered arrangement is very important, and the realized overall performance of the quantum dots is superior to that of any component material. However, in the existing research results of the lead sulfide quantum dots, the gravity center is mostly focused on how to reduce the size of the lead sulfide particles or improve performance indexes in subsequent device applications, but there are almost no reports on the ordered arrangement of the lead sulfide quantum dots, and the existing preparation methods cannot realize the controllable preparation of the ordered arrangement of the lead sulfide quantum dots.
Therefore, the development of a controllable preparation process route capable of realizing the ordered arrangement of the lead sulfide quantum dots has creative significance.
Disclosure of Invention
Aiming at the problems in the background art, the invention aims to provide a controllable preparation method of orderly-arranged lead sulfide quantum dots. The preparation method innovatively adopts a two-dimensional planar material with a grid structure as a template, and the controllable growth and ordered distribution of the lead sulfide quantum dots are realized by dispersing the lead sulfide sol on the two-dimensional material. The whole preparation method is simple and easy to realize, and quantum dots with uniform particle size distribution can be finally prepared.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a controllable preparation method of orderly-arranged lead sulfide quantum dots comprises the following steps:
step 1, preparing lead sulfide sol;
step 2, taking a two-dimensional plane material with a grid structure as a substrate, dripping the lead sulfide sol obtained in the step 1 to the center of the substrate, and then carrying out glue homogenizing treatment;
step 3, drying the substrate after the glue homogenizing treatment in the step 2;
and 4, repeating the step 2 and the step 3 for 5-12 times to obtain the orderly-arranged lead sulfide quantum dots.
Further, the specific process for preparing the lead sulfide sol in the step 1 is as follows:
step 1.1, dissolving a complexing agent into ethylene glycol, and uniformly stirring and mixing to obtain a solution A, wherein the volume ratio of the complexing agent to the ethylene glycol is 1: (8-15);
step 1.2, adding a lead source into the solution A prepared in the step, and stirring to obtain a solution B;
step 1.3, adding a sulfur source into an ethylene glycol solvent, and uniformly stirring and mixing to obtain a solution C, wherein the concentration of the sulfur source in the solution C is 0.1-1 mol/L;
step 1.4, adding the glycol solvent into the solution B prepared in the step 1.2 again to disperse the solution B again, stirring uniformly, standing for 20-40 min, and taking supernatant after standing;
step 1.5, dropwise adding the solution C obtained in the step 1.3 into the supernatant obtained in the step 1.4, and stirring the solution while dropwise adding to obtain a mixed solution D, wherein the molar ratio of lead ions to sulfur ions in the mixed solution D is (4-1): 1;
step 1.6, standing the mixed solution D obtained in the step 1.5 to settle large suspended particles to obtain a stable solution with uniform particle size distribution;
and 1.7, carrying out time chemical treatment on the solution subjected to standing treatment in the step 1.6 to prepare the required lead sulfide sol.
Further, the complexing agent in step 1.1 is ethylenediamine tetraacetic acid, triethylamine, butylamine, ethylenediamine and the like; the lead source in the step 1.2 is lead nitrate; the sulphur source in step 1.3 is sodium sulphide nonahydrate.
Further, the specific process of the time-based processing in step 1.7 is as follows: treating for 2-5 h at 80-120 ℃.
Further, in the step 2, the two-dimensional planar material with the grid structure is graphene, molybdenum disulfide, tungsten diselenide, hexagonal boron nitride, or the like.
Further, the specific parameters of the spin coating in step 3 are as follows: firstly, processing at a low speed of 400-700 rpm for 5-20 s; then, the high speed treatment is carried out at 3000-5000 rpm for 15-40 s.
Further, the drying process parameters in the step 4 are as follows: drying at 50-100 ℃ for 10-35 min.
The mechanism of the invention is as follows: graphene is a two-dimensional planar material with a lattice structure consisting of a single layer of carbon atoms, wherein the carbon atoms are sp2The hybrid orbit forms a honeycomb shape, the length of a C-C bond is about 0.142nm, the center of the grid structure of the graphene is exactly the place where the lead sulfide quantum dot is most stable, and ideally, one grid structure binds one quantum dot. Therefore, other two-dimensional planar materials with a lattice structure such as molybdenum disulfide, tungsten diselenide, hexagonal boron nitride should also work equally well.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the method takes a two-dimensional material with a grid structure as a substrate, and prepares the orderly-arranged lead sulfide quantum dots on the substrate by spin-coating lead sulfide sol. The preparation method realizes the ordered arrangement of the lead sulfide quantum dots by controlling the glue homogenizing parameters and the repetition times in the technical scheme.
2. The lead sulfide quantum dots prepared by the method are uniformly distributed and have special arrangement, the particle diameters are also uniformly distributed, and the particle diameters are concentrated near 28 nm.
Drawings
Fig. 1 is an SEM image of the lead sulfide quantum dots prepared in example 1 of the present invention.
Fig. 2 is a particle size distribution diagram of the lead sulfide quantum dots prepared in example 1 of the present invention.
Fig. 3 is an SEM image of the lead sulfide quantum dots prepared in comparative example 1.
Fig. 4 is an SEM image of the lead sulfide quantum dots prepared in comparative example 2.
Fig. 5 is an SEM image of the lead sulfide quantum dots prepared in comparative example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments and accompanying drawings.
Example 1
A controllable preparation method of orderly-arranged lead sulfide quantum dots comprises the following steps:
step 1, preparing lead sulfide sol, which comprises the following specific steps:
step 1.1, dissolving 4ml of triethylamine into ethylene glycol, and uniformly stirring and mixing to obtain a solution A, wherein the volume ratio of a complexing agent to the ethylene glycol is 1: 10;
step 1.2, adding 0.4mmol of lead nitrate into the solution A prepared in the step 1, and stirring to obtain a solution B;
step 1.3, adding 0.2mmol of sodium sulfide nonahydrate into an ethylene glycol solvent, and uniformly stirring and mixing to obtain a solution C, wherein the concentration of a sulfur source in the solution C is 0.1 mol/L;
step 1.4, adding 20ml of glycol solvent into the solution B prepared in the step 2 again to disperse the solution B again, stirring uniformly, standing for 30min, and taking supernatant after standing;
step 1.5, dropwise adding the solution C obtained in the step 3 into the supernatant obtained in the step 4, and stirring the solution while dropwise adding to obtain a mixed solution D, wherein the molar ratio of lead ions to sulfur ions in the mixed solution D is 2: 1;
step 1.6, standing the mixed solution D obtained in the step 5 for 3 hours to settle large suspended particles and obtain a stable solution with uniform particle size distribution;
step 1.7, performing time-varying treatment on the solution subjected to standing treatment in the step 6 at the temperature of 100 ℃ for 4 hours to prepare the required lead sulfide sol;
step 2, preparing a graphene substrate: cutting the graphene material to 5mm × 5mm, and adhering the graphene material on a carrying table by using a double-sided adhesive, wherein if the substrate is warped or bent, the spin coating effect may be affected;
and 3, dripping the lead sulfide sol obtained in the step 1 to the center of the graphene substrate obtained in the step 2 by using a dropper, and then carrying out glue homogenizing treatment, wherein the specific parameters are as follows: firstly processing at low speed of 550rpm/s for 15s, and then processing at high speed of 3000rpm/s for 30 s;
step 4, taking down the graphene substrate subjected to the glue homogenizing treatment in the step 3, and then putting the graphene substrate into an oven to be dried at the temperature of 60 ℃ for 20 min;
and 5, repeating the step 3 and the step 4 for 10 times to prepare the orderly-arranged lead sulfide quantum dots.
The SEM image of the lead sulfide quantum dot prepared in the example is shown in FIG. 1. As can be seen from fig. 1, the dots are lead sulfide quantum dots, the dark background in the figure is the graphene substrate, wherein the lead sulfide quantum dots are distributed orderly, that is, the lead sulfide quantum dots grow along the six-membered ring structure of the graphene substrate, and the particle diameters of the lead sulfide quantum dots are all concentrated near 28 nm.
Comparative example 1
Lead sulfide quantum dots in ordered arrangement are prepared according to the steps of example 1, and only the glue homogenizing parameters in the step 3 are adjusted as follows: firstly processing at low speed of 550rpm/s for 15s, then processing at high speed of 2500rpm/s for 30s, and other steps are not changed to prepare the required lead sulfide quantum dots.
The SEM image of the lead sulfide quantum dots prepared in the comparative example is shown in FIG. 3, and it can be seen from the SEM image that the glue homogenizing parameters play an important role in the preparation of the lead sulfide quantum dots which are orderly arranged.
Comparative example 2
And (3) preparing the orderly-arranged lead sulfide quantum dots according to the steps of the example 1, adjusting the repetition frequency in the step 5 to be 15 times, and keeping other steps unchanged to prepare the required lead sulfide quantum dots.
The SEM image of the lead sulfide quantum dots prepared in this comparative example is shown in fig. 4, and it can be seen from the figure that even under the condition of the same spin-coating parameters, if the difference of the number of repetitions is large, the lead sulfide quantum dots with ordered arrangement cannot be successfully prepared.
Comparative example 3
And (3) preparing the orderly-arranged lead sulfide quantum dots according to the steps of the example 1, and only adjusting the time-based treatment time in the step 1.7 to 1.5h, wherein other steps are unchanged, so that the required lead sulfide quantum dots are prepared.
The SEM image of the lead sulfide quantum dots prepared by the comparative example is shown in FIG. 5, and it can be seen from the SEM image that the obtaining of lead sulfide sol is also a key factor for successfully preparing the orderly-arranged lead sulfide quantum dots.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.
Claims (4)
1. A controllable preparation method of orderly-arranged lead sulfide quantum dots is characterized by comprising the following steps:
step 1, preparing lead sulfide sol, which comprises the following specific steps:
step 1.1, dissolving a complexing agent into ethylene glycol, and uniformly stirring and mixing to obtain a solution A, wherein the volume ratio of the complexing agent to the ethylene glycol is 1: (8-15);
step 1.2, adding a lead source into the solution A prepared in the step 1.1, and stirring to obtain a solution B;
step 1.3, adding a sulfur source into an ethylene glycol solvent, and uniformly stirring and mixing to obtain a solution C, wherein the concentration of the sulfur source in the solution C is 0.1-1 mol/L;
step 1.4, adding the glycol solvent into the solution B prepared in the step 1.2 again to disperse the solution B again, stirring uniformly, standing for 20-40 min, and taking supernatant after standing;
step 1.5, dropwise adding the solution C obtained in the step 1.3 into the supernatant obtained in the step 1.4, and stirring the solution while dropwise adding to obtain a mixed solution D, wherein the molar ratio of lead ions to sulfur ions in the mixed solution D is (4-1): 1;
step 1.6, standing the mixed solution D obtained in the step 1.5 to settle large suspended particles;
step 1.7, carrying out time-based treatment on the solution subjected to standing treatment in the step 1.6 at the temperature of 80-120 ℃, and treating for 2-5 hours to obtain the required lead sulfide sol;
and 2, taking a two-dimensional plane material with a grid structure as a substrate, dripping the lead sulfide sol obtained in the step 1 to the center of the substrate, and then carrying out glue homogenizing treatment, wherein the specific parameters of the glue homogenizing treatment are as follows: firstly, processing at a low speed of 400-700 rpm for 5-20 s; then processing at a high speed of 3000-5000 rpm for 15-40 s;
step 3, drying the substrate after the glue homogenizing treatment in the step 2;
and 4, repeating the step 2 and the step 3 for 5-12 times to obtain the orderly-arranged lead sulfide quantum dots.
2. The controllable preparation method of lead sulfide quantum dots as claimed in claim 1, wherein the complexing agent in step 1.1 is ethylenediamine tetraacetic acid, triethylamine, butylamine, or ethylenediamine; the lead source in the step 1.2 is lead nitrate; the sulphur source in step 1.3 is sodium sulphide nonahydrate.
3. The controllable preparation method of lead sulfide quantum dots according to claim 1, wherein the two-dimensional planar material with the grid structure in the step 2 is graphene, molybdenum disulfide, tungsten diselenide or hexagonal boron nitride.
4. The controllable preparation method of the lead sulfide quantum dot as claimed in claim 1, wherein the drying process parameters in the step 3 are as follows: drying at 50-100 ℃ for 10-35 min.
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