CN111635759B - Preparation method of lead sulfide colloidal quantum dots - Google Patents
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Abstract
The invention belongs to the synthesis of semiconductor nano particles, and particularly relates to a preparation method of lead sulfide colloidal quantum dots. The synthesis method comprises the following steps: the method comprises the steps of taking submicron-grade basic lead chloride synthesized by an aqueous solution precipitation method as a lead source, heating the submicron-grade basic lead chloride and an organic reagent to form a lead precursor solution, then injecting a simple substance sulfur solution dissolved in oleylamine into the lead precursor solution at a specific temperature to react for 0.5-20 min to obtain a lead sulfide colloidal quantum dot stock solution, and finally obtaining the lead sulfide colloidal quantum dot solution after impurity removal and purification by an anti-solvent method. The synthesis method disclosed by the invention has the advantages of good controllability, stable chemical properties of reactant raw materials, high fluorescence efficiency of reaction products and the like, and is suitable for batch synthesis of high-quality lead sulfide colloid quantum dots.
Description
Technical Field
The invention belongs to the field of preparation of semiconductor nano materials, and particularly relates to a preparation method of lead sulfide colloidal quantum dots.
Background
The quantum dots are a kind of semiconductor nanocrystals with three-dimensional size smaller than the Bohr radius, have quantum confinement effect, and the light emitting/light absorbing range can be adjusted by controlling the size of the nanocrystals. The lead sulfide (PbS) quantum dots have the characteristic of continuously adjustable optical performance in the near-infrared wavelength range, and are widely applied to numerous fields such as solar cells, photoluminescence diodes, biological imaging and infrared image sensors as key materials. In the application process, the quality of the quantum dots plays a crucial role in the performance of the corresponding device, and the quality mainly depends on the synthesis process of the quantum dots.
At the present stage, a thermal injection method is usually adopted for preparing the lead sulfide quantum dots, specifically, another precursor solution is rapidly injected into a high-temperature high-boiling-point precursor solution, chemical reaction occurs between precursors, the monomer concentration is supersaturated to initiate instant nucleation, and simultaneously, along with the injection of the precursor solution with lower temperature, the temperature of a reaction system is reduced, and nanoparticles enter a growth state. Finally, the reaction can be stopped by rapid cooling. During the synthesis process, the selection of raw materials is crucial to the design of the reaction process and the influence of the reaction result. The sulfur sources mainly adopted in the current hot injection synthesis approach are hexamethyldisilazane (TMS), thiourea and simple substance S. The method using TMS and thiourea as sulfur sources can synthesize PbS quantum dots in a wider range, and elemental S has the most stable chemical property and low requirements on synthesis conditions. Although they can synthesize high-quality quantum dots, they have a problem of poor reproducibility of the result due to poor controllability.
Disclosure of Invention
The invention provides a preparation method of lead sulfide colloid quantum dots, aiming at solving the problems of complex synthesis process and poor result repeatability of quantum dots. The reaction is a top-down process, and the micron/submicron basic lead chloride is directly crushed by ion replacement, and PbS quantum dots are generated at the same time. The process has no participation of nucleation reaction, is beneficial to controlling the growth of PbS quantum dots and improving the reproducibility of reaction results; on the other hand, different from the conventional synthesis way, the basic lead chloride can react with S according to the molar ratio of 1:1, so that the waste of lead precursors is avoided, and the pollution of residual lead sources to the environment is reduced. The obtained quantum dots have high fluorescence efficiency and good chemical/light stability and have good application prospect. The method comprises the following steps:
(1) respectively weighing sodium chloride and basic lead acetate to prepare aqueous solution with certain concentration; then mixing the two solutions, reacting at a certain temperature for 10-60 min, washing the obtained white precipitate with distilled water, and drying to remove water to obtain basic lead chloride;
(2) under the protection of nitrogen, heating and reacting the basic lead chloride synthesized in the step (1) with an organic reagent at 90-160 ℃ for 30min, and then vacuumizing for 30min to obtain a lead precursor solution;
(3) mixing elemental sulfur and oleylamine at normal temperature to prepare a sulfur precursor solution with a certain concentration; then, quickly injecting a certain volume of sulfur precursor solution into the lead precursor solution with the nitrogen protection recovered and the set temperature in the step (2); finally, reacting at constant temperature for 0.5-20 min, cooling to 10-20 ℃, and stopping reaction to obtain lead sulfide colloidal quantum dot stock solution;
(4) and (4) centrifuging the quantum dot stock solution prepared in the step (3) to remove impurities, diluting with a quantum dot solvent, purifying the quantum dot solution with a strong-polarity organic solvent, centrifuging again, and re-dissolving the separated solid quantum dots in a specific solvent to obtain a lead sulfide colloidal quantum dot solution.
More preferably, the concentration of the sodium chloride and the basic lead acetate in the step (1) is 0.2M-2M; the reaction temperature in the step (1) is 25-90 ℃; the basic lead chloride in the step (1) has any morphology with micron or submicron size;
preferably, the organic reagent in the step (2) is at least two of octylamine, oleylamine, oleic acid and octadecene; and (3) the lead precursor solution in the step (2) is a clear solution when reacting with the S solution.
Preferably, the concentration of the sulfur precursor solution in the step (3) is 0.1M-0.5M; the temperature of the lead precursor in the step (3) is 60-160 ℃ during sulfur injection;
preferably, the quantum dot solvent in the step (4) is one of toluene, chloroform and hexane; the polar organic solvent in the step (4) is at least one of methanol, ethanol, butanol and acetone, preferably ethanol and acetone; the specific solvent in the step (4) is at least one of toluene, chloroform, hexane, decane and decene; the first exciton absorption peak range of the PbS colloid quantum dots in the step (4) is 950nm-1800nm.
Compared with the prior art, the invention has the beneficial effects that:
(1) the size or absorption peak of the quantum dot is easy to control, and the reaction result has good reproducibility;
(2) the raw materials used are stable in chemical property and easy to store;
(3) the prepared quantum dots have high fluorescence efficiency;
(4) different from the conventional synthesis process that the lead source needs to be excessive, the method provided by the invention is suitable for synthesizing the PbS quantum dots by reacting according to the lead-sulfur ratio of 1:1, and avoids the waste of the lead source and the environmental pollution caused by the process.
Detailed Description
The following provides a more detailed description of the preparation process of the present invention with reference to specific examples. It should be understood that the following examples are only for illustrating the present invention, and the implementation method of the changes or improvements made by the technical idea of the present invention is within the protection scope of the appended claims.
Example 1
A: 1.2g of sodium chloride and 6g of basic lead acetate (Pb (CH)3COO)2·Pb(OH)2) And dissolved in 15ml of distilled water respectively to prepare 1.37M solution and 0.7M solution; then mixing the two solutions, reacting for 15min at 80 ℃, washing the obtained white precipitate with distilled water, and drying to remove water to obtain basic lead chloride; weighing 0.278g (0.001mol) of synthesized basic lead chloride and 15ml of octylamine/oleic acid/octadecene mixed reagent, heating and reacting for 30min at 130 ℃ under the protection of nitrogen, and vacuumizing for 30min to obtain a lead precursor solution;
b: 0.032g (0.001mol) of elemental sulfur and 3.5ml of oleylamine are mixed at normal temperature and rapidly dissolved under the ultrasonic action to obtain 0.286M sulfur precursor solution; then, rapidly injecting the sulfur precursor solution into the lead precursor solution which is cooled to 70 ℃ and is obtained in the step A under the nitrogen atmosphere; finally, reacting at constant temperature for 30s, cooling to 15 ℃, and stopping the reaction to obtain a lead sulfide colloidal quantum dot stock solution;
c: centrifuging the colloidal quantum dot stock solution prepared in the step B to remove unreacted impurities, and transferring the obtained supernatant to a new container to mix with toluene with 2 times of volume; then, ethanol is added to purify the quantum dot solution, the solution is centrifuged again, and the solid quantum dots obtained after separation are dissolved in toluene again to obtain a lead sulfide colloidal quantum dot solution (table 1) with a first exciton absorption peak position of 1350nm and a fluorescence efficiency of 62%.
Example 2
A: 1.2g of sodium chloride and 6g of basic lead acetate (Pb (CH)3COO)2·Pb(OH)2) And dissolved in 15ml of distilled water respectively to prepare 1.37M solution and 0.7M solution; then mixing the two solutions, reacting for 15min at 80 ℃, washing the obtained white precipitate with distilled water, and drying to remove water to obtain basic lead chloride; 0.278g (0.001mol) of synthesized basic lead chloride and 15ml of oleylamine/oleic acid/octadecene mixed reagent are weighed, heated and reacted for 30min at 130 ℃ under the protection of nitrogen, and then pumped outVacuum for 30min to obtain lead precursor solution;
b: 0.032g (0.001mol) of elemental sulfur and 3.5ml of oleylamine are mixed at normal temperature and rapidly dissolved under the ultrasonic action to obtain 0.286M sulfur precursor solution; then quickly injecting the sulfur precursor solution into the lead precursor solution which is cooled to 90 ℃ and is obtained in the step A under the nitrogen atmosphere; finally, reacting at constant temperature for 30s, cooling to 15 ℃, and stopping the reaction to obtain a lead sulfide colloidal quantum dot stock solution;
c: centrifuging the colloidal quantum dot stock solution prepared in the step B to remove unreacted impurities, and transferring the obtained supernatant to a new container to mix with toluene with 2 times of volume; then, ethanol is added to purify the quantum dot solution, the solution is centrifuged again, and the solid quantum dots obtained after separation are dissolved in toluene again to obtain a lead sulfide colloidal quantum dot solution (table 1) with the first exciton absorption peak position of 1565nm and the fluorescence efficiency of 55%.
Example 3
A: 1.2g of sodium chloride and 6g of basic lead acetate (Pb (CH)3COO)2·Pb(OH)2) And dissolved in 15ml of distilled water respectively to prepare 1.37M solution and 0.7M solution; then mixing the two solutions, reacting for 15min at 80 ℃, washing the obtained white precipitate with distilled water, and drying to remove water to obtain basic lead chloride; weighing 0.278g (0.001mol) of the synthesized basic lead chloride, mixing with 15ml of octylamine/oleic acid/octadecene mixed reagent, heating and reacting for 30min at 130 ℃ under the protection of nitrogen, and vacuumizing for 30min to obtain a lead precursor solution;
b: 0.032g (0.001mol) of elemental sulfur and 3.5ml of oleylamine are mixed at normal temperature and rapidly dissolved under the ultrasonic action to obtain 0.286M sulfur precursor solution; then, rapidly injecting the sulfur precursor solution into the lead precursor solution which is cooled to 120 ℃ and is obtained in the step A under the nitrogen atmosphere; finally, reacting at constant temperature for 10min, cooling to 15 ℃, and stopping the reaction to obtain a lead sulfide colloidal quantum dot stock solution;
c: centrifuging the colloidal quantum dot stock solution prepared in the step B to remove unreacted impurities, and transferring the obtained supernatant to a new container to mix with toluene with 2 times of volume; then, ethanol is added to purify the quantum dot solution, the solution is centrifuged again, and the solid quantum dots obtained after separation are re-dissolved in toluene to obtain a lead sulfide colloidal quantum dot solution (table 1) with a first exciton absorption peak position of 1663nm and a fluorescence efficiency of 31%.
Example 4
A: 1.2g of sodium chloride and 6g of basic lead acetate (Pb (CH)3COO)2·Pb(OH)2) And dissolved in 15ml of distilled water respectively to prepare 1.37M solution and 0.7M solution; then mixing the two solutions, reacting for 15min at 80 ℃, washing the obtained white precipitate with distilled water, and drying to remove water to obtain basic lead chloride; weighing 0.278g (0.001mol) of the synthesized basic lead chloride, mixing with 15ml of oleylamine/oleic acid/octadecene mixed reagent, heating and reacting for 30min at 130 ℃ under the protection of nitrogen, and vacuumizing for 30min to obtain a lead precursor solution;
b: 0.032g (0.001mol) of elemental sulfur and 3.5ml of oleylamine are mixed at normal temperature and rapidly dissolved under the ultrasonic action to obtain 0.286M sulfur precursor solution; then, rapidly injecting the sulfur precursor solution into the lead precursor solution which is cooled to 160 ℃ and is obtained in the step A under the nitrogen atmosphere; finally, reacting for 15min at constant temperature, cooling to 15 ℃, and stopping the reaction to obtain a lead sulfide colloidal quantum dot stock solution;
c: centrifuging the colloidal quantum dot stock solution prepared in the step B to remove unreacted impurities, and transferring the obtained supernatant to a new container to mix with toluene with 2 times of volume; then, ethanol is added to purify the quantum dot solution, the solution is centrifuged again, and the solid quantum dots obtained after separation are dissolved in toluene again to obtain a lead sulfide colloidal quantum dot solution (table 1) with a first exciton absorption peak position of 1780nm and a fluorescence efficiency of 30%.
Example 5
A: 1.2g of sodium chloride and 6g of basic lead acetate (Pb (CH)3COO)2·Pb(OH)2) And dissolved in 15ml of distilled water respectively to prepare 1.37M solution and 0.7M solution; then mixing the two solutions, reacting for 15min at 80 ℃, washing the obtained white precipitate with distilled water, and drying to remove water to obtain basic lead chloride; 0.278g (0.001mol) of the synthesized basic lead chloride was weighed out and mixed with 15ml of octylamine/oleic acid/octadecene mixed reagent under nitrogen atmosphereHeating and reacting at 160 ℃ for 30min under protection, and vacuumizing for 30min to obtain a lead precursor solution;
b: 0.032g (0.001mol) of elemental sulfur and 3.5ml of oleylamine are mixed at normal temperature and rapidly dissolved under the ultrasonic action to obtain 0.286M sulfur precursor solution; then, rapidly injecting the sulfur precursor solution into the lead precursor solution which is cooled to 70 ℃ and is obtained in the step A under the nitrogen atmosphere; finally, reacting at constant temperature for 30s, cooling to 15 ℃, and stopping the reaction to obtain a lead sulfide colloidal quantum dot stock solution;
c: centrifuging the colloidal quantum dot stock solution prepared in the step B to remove unreacted impurities, and transferring the obtained supernatant to a new container to mix with toluene with 2 times of volume; then, ethanol is added to purify the quantum dot solution, the solution is centrifuged again, and the solid quantum dots obtained after separation are dissolved in toluene again to obtain a lead sulfide colloidal quantum dot solution (shown in table 1) with a first exciton absorption peak position of 1162nm and a fluorescence efficiency of 65%.
Example 6
A: 1.2g of sodium chloride and 6g of basic lead acetate (Pb (CH)3COO)2·Pb(OH)2) And dissolved in 15ml of distilled water respectively to prepare 1.37M solution and 0.7M solution; then mixing the two solutions, reacting for 15min at 80 ℃, washing the obtained white precipitate with distilled water, and drying to remove water to obtain basic lead chloride; weighing 0.278g (0.001mol) of the synthesized basic lead chloride, mixing with 15ml of oleylamine/oleic acid mixed reagent, heating and stirring at 160 ℃ for 30min under the protection of nitrogen, and vacuumizing for 30min to obtain a lead precursor solution;
b: 0.032g (0.001mol) of elemental sulfur and 3.5ml of oleylamine are mixed at normal temperature and rapidly dissolved under the ultrasonic action to obtain 0.286M sulfur precursor solution; then, rapidly injecting the sulfur precursor solution into the lead precursor solution which is cooled to 70 ℃ and is obtained in the step A under the nitrogen atmosphere; finally, reacting at constant temperature for 30s, cooling to 15 ℃, and stopping the reaction to obtain a lead sulfide colloidal quantum dot stock solution;
c: centrifuging the colloidal quantum dot stock solution prepared in the step B to remove unreacted impurities, and transferring the obtained supernatant to a new container to mix with toluene with 2 times of volume; then, ethanol is added to purify the quantum dot solution, the solution is centrifuged again, and the separated solid quantum dots are re-dissolved in toluene to obtain a lead sulfide colloidal quantum dot solution (table 1) with a first exciton absorption peak position of 1440nm and a fluorescence efficiency of 60%.
TABLE 1 first exciton absorption peak position of PbS colloidal quantum dots synthesized by each example
The foregoing merely represents preferred embodiments of the invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (2)
1. A preparation method of lead sulfide colloidal quantum dots is characterized in that alkaline lead chloride in any shape of micron or submicron order synthesized by an aqueous solution precipitation method is used as a lead source, and the alkaline lead chloride and elemental sulfur are subjected to an anion displacement reaction to synthesize the lead sulfide colloidal quantum dots, wherein the reaction is a top-down process without participation of a nucleation reaction, and the method specifically comprises the following steps:
(1) respectively weighing sodium chloride and basic lead acetate to prepare aqueous solution with certain concentration; then mixing the two solutions, reacting at a certain temperature for 10-60 min, washing the obtained white precipitate with distilled water, and drying to remove water to obtain basic lead chloride; the concentration of the sodium chloride and the basic lead acetate is 0.2M-2M; the reaction temperature is 25-90 ℃; the basic lead chloride has any morphology with micron or submicron size;
(2) under the protection of nitrogen, heating and reacting the basic lead chloride synthesized in the step (1) with an organic reagent at 90-160 ℃ for 30min, and then vacuumizing for 30min to obtain a lead precursor solution; the organic reagent is at least two of octylamine, oleylamine, oleic acid and octadecene; the lead precursor solution is a clear solution when reacting with the sulfur precursor solution;
(3) mixing elemental sulfur and oleylamine at normal temperature to prepare a sulfur precursor solution with a certain concentration; then, quickly injecting a certain volume of sulfur precursor solution into the lead precursor solution with the nitrogen protection recovered and the set temperature in the step (2); finally, reacting at constant temperature for 0.5-20 min, cooling to 10-20 ℃, and stopping reaction to obtain lead sulfide colloidal quantum dot stock solution; the concentration of the sulfur precursor solution is 0.1M-0.5M; wherein the temperature of the lead precursor is 60-160 ℃ when the sulfur precursor is injected;
(4) and (3) centrifuging the quantum dot stock solution prepared in the step (3) to remove impurities, diluting with a quantum dot solvent, purifying the quantum dot solution with a polar organic solvent, centrifuging again, and re-dissolving the separated solid quantum dots in a specific solvent to obtain a lead sulfide colloidal quantum dot solution, wherein the polar organic solvent is at least one of methanol, ethanol, butanol and acetone.
2. The method for preparing lead sulfide colloidal quantum dots according to claim 1, wherein the method comprises the following steps: the quantum dot solvent in the step (4) is one of toluene, chloroform and hexane; the specific solvent in the step (4) is at least one of toluene, chloroform, hexane, decane and decene; the first exciton absorption peak range of the PbS colloid quantum dots in the step (4) is 1000 nm-1800nm.
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