CN111635759B - Preparation method of lead sulfide colloidal quantum dots - Google Patents

Preparation method of lead sulfide colloidal quantum dots Download PDF

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CN111635759B
CN111635759B CN202010548804.0A CN202010548804A CN111635759B CN 111635759 B CN111635759 B CN 111635759B CN 202010548804 A CN202010548804 A CN 202010548804A CN 111635759 B CN111635759 B CN 111635759B
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谭龙
谭恋
汤昊
孙润光
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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

Preparation method of lead sulfide colloidal quantum dots
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
Figure BDA0002541742950000061
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)

1.一种硫化铅胶体量子点的制备方法，其特征在于，以水溶液沉淀法所合成的微米或亚微米级的任意形貌的碱式氯化铅为铅源，与单质硫进行阴离子置换反应合成硫化铅胶体量子点的途径，该反应是一种自上而下的过程，无成核反应的参与，具体包括如下步骤：1. a preparation method of lead sulfide colloidal quantum dots, is characterized in that, the basic lead chloride of the arbitrary morphology of micron or submicron level synthesized by aqueous solution precipitation method is lead source, carries out anion replacement reaction with elemental sulfur The method for synthesizing lead sulfide colloidal quantum dots, the reaction is a top-down process without the participation of nucleation reaction, and specifically includes the following steps: （1）分别称取氯化钠和碱式乙酸铅配制成一定浓度的水溶液；然后将两种溶液混合并在一定温度下反应10 min-60 min，所得白色沉淀用蒸馏水冲洗并干燥去除水分得碱式氯化铅；所述氯化钠和碱式乙酸铅的浓度为0.2 M-2 M；所述反应的温度为25 ℃-90 ℃；所述碱式氯化铅具有微米或亚微米尺寸的任意形貌；(1) Weigh sodium chloride and basic lead acetate respectively to prepare an aqueous solution of a certain concentration; then mix the two solutions and react at a certain temperature for 10 min-60 min, the obtained white precipitate is rinsed with distilled water and dried to remove moisture. Basic lead chloride; the concentration of the sodium chloride and basic lead acetate is 0.2 M-2 M; the temperature of the reaction is 25 ℃-90 ℃; the basic lead chloride has a micron or submicron size any shape of ; （2）在氮气保护下，将步骤（1）所合成的碱式氯化铅与有机试剂在90 ℃-160 ℃加热反应30 min后，然后抽真空30 min得铅前驱体溶液；所述有机试剂为辛胺，油胺，油酸，十八烯中的至少两种；所述铅前驱体溶液在与硫前驱体溶液反应时为澄清溶液；(2) Under the protection of nitrogen, the basic lead chloride synthesized in step (1) and the organic reagent are heated and reacted at 90 ℃-160 ℃ for 30 minutes, and then vacuumized for 30 minutes to obtain a lead precursor solution; The reagents are 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）将单质硫与油胺在常温下混合配制成一定浓度的硫前驱体溶液；然后把一定体积的硫前驱体溶液快速注入步骤（2）中恢复氮气保护以及设定好温度的铅前驱体溶液中；最后，经恒温反应0.5 min-20 min后冷却至10-20 ℃停止反应得到硫化铅胶体量子点原液；所述硫前驱体溶液浓度为0.1 M-0.5 M；其中的硫前驱体注射时铅前驱体温度为60 ℃-160℃；(3) Mix elemental sulfur and oleyl amine at room temperature to prepare a sulfur precursor solution of a certain concentration; then inject a certain volume of sulfur precursor solution into step (2) to restore nitrogen protection and set the temperature of the lead precursor In the bulk solution; finally, after constant temperature reaction for 0.5 min-20 min, cooling to 10-20 °C to stop the reaction to obtain lead sulfide colloidal quantum dots stock solution; the concentration of the sulfur precursor solution is 0.1 M-0.5 M; The temperature of lead precursor during injection is 60 ℃-160 ℃; （4）将步骤（3）制备的量子点原液经离心去除杂质后，再用量子点溶剂进行稀释，然后以极性有机溶剂对量子点溶液进行纯化，再次离心，将分离后得到的固体量子点重新溶解在特定溶剂中得到硫化铅胶体量子点溶液，所述极性有机溶剂为甲醇，乙醇，丁醇以及丙酮中的至少一种。(4) After centrifuging the quantum dot stock solution prepared in step (3) to remove impurities, dilute it with a quantum dot solvent, and then purify the quantum dot solution with a polar organic solvent, centrifuge again, and separate the solid quantum dots obtained after separation. The dots are redissolved in a specific solvent to obtain a lead sulfide colloidal quantum dot solution, and the polar organic solvent is at least one of methanol, ethanol, butanol and acetone. 2.根据权利要求1所述的一种硫化铅胶体量子点的制备方法，其特征在于：所述步骤（4）中的量子点溶剂为甲苯，氯仿，己烷中的一种；所述步骤（4）中的特定溶剂为甲苯，氯仿，己烷，癸烷以及癸烯中的至少一种；所述步骤（4）中的PbS胶体量子点第一激子吸收峰范围为1000 nm-1800 nm。2 . The method for preparing lead sulfide colloidal quantum dots according to claim 1 , wherein the quantum dot solvent in the step (4) is one of toluene, chloroform and hexane; the step The specific solvent in (4) is at least one of toluene, chloroform, hexane, decane and decene; the first exciton absorption peak range of the PbS colloidal quantum dots in the step (4) is 1000 nm-1800 nm.
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