CN106398686B - Quantum dot and preparation method thereof - Google Patents
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Abstract
The invention discloses a quantum dot and a preparation method thereof, wherein the method comprises the following steps: firstly, preparing a solid fiber membrane, then placing the prepared solid fiber membrane into a cation precursor solution for crosslinking, and then injecting an anion precursor into the crosslinked solid fiber membrane for reaction to obtain quantum dots; wherein the size of the solid fiber membrane is nano-scale or micron-scale. The invention takes the solid-state nano fiber as the microreactor, the reaction temperature is lower, the quantum dot can rapidly nucleate and grow at a solid-liquid interface, and the size of the quantum dot can be adjusted by controlling the size of the solid-state fiber membrane or the reaction temperature. In addition, the solid-state nanofiber membrane used as the microreactor can be repeatedly utilized, so that the cost is greatly saved. In addition, the method is simple to operate, easy to repeat and can be used for preparing the oil-soluble quantum dots.
Description
Technical Field
The invention relates to the field of quantum dot synthesis, in particular to a quantum dot and a preparation method thereof.
Background
In recent years, researchers have extensively studied the optical properties of quantum dots due to the tremendous applicability of colloidal quantum dots in biosensing, biomarkers, and light emitting diodes. Due to the requirements on the structure and performance of luminescent quantum dots, the controllable synthesis thereof has become an interesting research area.
In the synthesis of luminescent quantum dots, researchers have developed a variety of preparation methods, such as metal-organic precursor methods, solvothermal methods, aqueous phase synthesis methods, ion beam synthesis methods, ultrasonic irradiation methods, thermal implantation methods, chemical water bath deposition methods, microwave-assisted chemical water bath deposition methods, and solvent growth methods. The most widely used preparation method is a thermal injection method, in which an anion precursor of Se, S, Te and the like is injected into a cation precursor of Cd, Zn, Pb and the like at high temperature to rapidly growNucleation and then crystal growth at a certain temperature to form quantum dots. However, the quantum dots prepared by the above method require reaction in a uniform system and can be reacted at a relatively high temperature (generally above 280 ℃). In recent years, the liquid-liquid two-phase method is gradually developed and used for quantum dot synthesis, mainly nucleation and crystal growth are carried out at a water-oil phase interface. Compared with the traditional thermal injection method, the method can carry out reaction at a lower temperature (generally lower than 200 ℃) to synthesize quantum dots with uniform size. However, the liquid-liquid two-phase method still has certain defects, the cation precursor required by the method is generally long-chain alkyl acid metal salt, the oil phase is generally produced by adopting toluene, which is a toxic solvent, and in order to ensure that the generated quantum dots enter the oil phase from the two-phase interface in the reaction process, long-chain hydrocarbon (C) is also required to be added6-C18) As a wrapping agent. In addition, this process, although allowing the reaction to be carried out at relatively low temperatures, requires high pressures as an auxiliary condition.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention provides a quantum dot and a preparation method thereof, aiming at solving the problem of the defects of the liquid-liquid two-phase method in the prior art.
The technical scheme of the invention is as follows:
a preparation method of quantum dots comprises the following steps: firstly, preparing a solid fiber membrane, then placing the prepared solid fiber membrane into a cation precursor solution for crosslinking, and then injecting an anion precursor into the crosslinked solid fiber membrane for reaction to obtain quantum dots; wherein the size of the solid fiber membrane is nano-scale or micron-scale.
The preparation method of the quantum dot comprises the step of preparing a solid fiber membrane, wherein the solid fiber membrane is one of a sodium citrate fiber membrane, a potassium citrate fiber membrane, a sodium alginate fiber membrane, a potassium alginate fiber membrane, a calcium alginate fiber membrane, a silicon dioxide fiber membrane and a titanium dioxide fiber membrane.
The preparation method of the quantum dot comprises the step of preparing the solid fiber membrane by an electrostatic spinning method.
The preparation method of the quantum dot comprises the step of reacting the anion precursor and the cation precursor at a solid-liquid interface at a temperature of 120-160 ℃.
The preparation method of the quantum dot comprises the step of dissolving a cation precursor in a solvent to prepare the cation precursor solution.
The preparation method of the quantum dot comprises the step of preparing the cation precursor CdCl2、ZnCl2、Cd(NO3)2、Zn(NO3)2、Pb(NO3)2、Cd(Ac)2、Zn(Ac)2、Pb(Ac)2One or more of (a).
The preparation method of the quantum dot comprises the step of preparing a cation precursor solution by using a solvent, wherein the solvent of the cation precursor solution is ethanol.
The preparation method of the quantum dot comprises the following step of preparing an anion precursor, wherein the anion precursor is one or more of S-ODE, S-TOP, S-TOPO, S-OA, S-OLA, S-TBP, S-DDA, Se-ODE, Se-TOP, Se-TOPO and Se-TBP.
A quantum dot is prepared by the preparation method of the quantum dot.
The quantum dots are CdS, CdSe, ZnSe, ZnS, PbSe, PbS, CdTe and Cd1- xZnxS、Cd1-xZnxSe、CdSeyS1-y、Cd1-xZnxSeyS1-y、PbSeXS1-X、ZnXCd1-XOne of Te, wherein x is more than or equal to 0<1，0≤y≤1。
Has the advantages that: the invention takes the solid fiber membrane as a micro-reactor to prepare the oil-soluble quantum dots at a lower temperature. The solid fiber membrane adopts a micron/nano-scale solid fiber membrane, so that the anion precursor and the cation precursor can be rapidly and completely mixed at a solid-liquid interface in a short time, and quickly react to generate quantum dots. In addition, the solid-state nanofiber membrane used as the microreactor can be repeatedly utilized, so that the cost is greatly saved.
Drawings
Fig. 1 is a schematic diagram of a quantum dot preparation method according to an embodiment of the present invention.
Detailed Description
The present invention provides a quantum dot and a method for preparing the same, and the present invention is further described in detail below in order to make the objects, technical solutions, and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The preferred embodiment of the preparation method of the quantum dot comprises the following steps: firstly, preparing a solid fiber membrane, then placing the prepared solid fiber membrane into a cation precursor solution for crosslinking, and then injecting an anion precursor into the crosslinked solid fiber membrane for reaction to obtain quantum dots; wherein the size of the solid fiber membrane is nano-scale or micron-scale.
The invention takes the nano-scale or micron-scale solid fiber membrane as the microreactor, so that the anion and cation precursors can rapidly react at the solid-liquid interface in a short time to prepare the quantum dots. The micron-level or nano-level solid fiber membrane has the characteristics of small reaction space, large specific surface area, high surface activity and the like, and can ensure that quantum dots rapidly nucleate and grow at a solid-liquid interface. The raw materials adopted by the method are relatively common metal salts, no specific metal-organic compound is needed, the reaction temperature of the anion precursor and the cation precursor at the solid-liquid interface can be 120-160 ℃ (such as 130 ℃ or 140 ℃), namely the reaction can be carried out at a lower temperature, and the size of the quantum dot can be adjusted through the size of the solid fiber film or the reaction temperature. In addition, the solid fiber membrane used as the microreactor can be repeatedly utilized, so that the cost is greatly saved.
Preferably, the solid fiber membrane of the present invention may be one of a sodium citrate fiber membrane, a potassium citrate fiber membrane, a sodium alginate fiber membrane, a potassium alginate fiber membrane, a calcium alginate fiber membrane, a silica fiber membrane, a titanium dioxide fiber membrane, and the like. The solid fiber membranes can be used as microreactors, and the sizes of the microreactors are all nano-scale or micro-scale. More preferably, the solid fibrous membrane is a sodium citrate fibrous membrane or a potassium citrate fibrous membrane.
Preferably, the present invention can prepare a solid fiber membrane by an electrospinning method. For example, sodium citrate fiber membranes can be prepared by electrospinning.
The cation precursor solution is prepared by dissolving a cation precursor in a solvent (such as ethanol). Preferably, the cationic precursor may be CdCl2、ZnCl2、Cd(NO3)2、Zn(NO3)2、Pb(NO3)2、Cd(Ac)2、Zn(Ac)2、Pb(Ac)2And the like. More preferably, the cationic precursor is CdCl2Or ZnCl2。
Preferably, the anion precursor is one or more of S-ODE, S-TOP, S-TOPO, S-OA, S-OLA, S-TBP, S-DDA, Se-ODE, Se-TOP, Se-TOPO, Se-TBP and the like. Wherein S-ODE, S-TOP, S-TOPO, S-OA, S-OLA, S-TBP, S-DDA, Se-ODE, Se-TOP, Se-TOPO, Se-TBP and the like mean that S or Se powder is dissolved in corresponding organic matters, namely S is dissolved in ODE, S is dissolved in TOP, and Se is dissolved in ODE and the like.
Based on the method, the invention provides the quantum dot which is prepared by adopting the preparation method of the quantum dot. The quantum dots can be CdS, CdSe, ZnSe, ZnS, PbSe, PbS, CdTe and Cd1-xZnxS、Cd1-xZnxSe、CdSeyS1-y、Cd1-xZnxSeyS1-y、PbSeXS1-X、ZnXCd1-XTe, etc., wherein 0 is less than or equal to x<1，0≤y≤1。
The present invention will be described in detail below with reference to examples.
Example 1
Referring to fig. 1, the quantum dots are prepared as follows:
(1) the sodium citrate fiber membrane is prepared by an electrostatic spinning method
3g of sodium citrate was dissolved in 10mL of distilled water, 3wt% of dimethylethylsulfone was added as a cosolvent, 2.4g of polystyrene was added, and then stirred at 60 ℃ for 3 hours to obtain a uniform solution. The solution was injected into a 10mL syringe using a stainless steel needle with an inner diameter of 0.4mm as the solution injection tip. A4 cm-5 cm copper net is used as a collector, the distance from a spraying needle to the copper net is 12cm, and an ultraviolet lamp with the power of 100W is used for irradiation in the middle. The spraying speed of the solution was 1.2mL/h, and the high voltage power supply was 18 kV. Obtaining a nano-scale sodium citrate fiber membrane with a certain thickness after the whole spinning process lasts for 4 hours, taking down the sodium citrate fiber membrane from the copper mesh, and placing the sodium citrate fiber membrane in N2Keeping the temperature in an atmosphere furnace at 80 ℃ for 6h, and cooling to room temperature for later use.
(2) Cross-linking of cationic precursor with sodium citrate fibrous membranes
Zn (NO) in a concentration of 2mmol/mL3)2And 0.2mmol/mL Cd (NO)3)2The sodium citrate fiber membrane prepared by electrostatic spinning is put into the ethanol solution to be soaked for 2 hours, so that the sodium citrate fiber membrane is fully crosslinked. And after the sodium citrate fiber membrane is fully soaked, taking out the sodium citrate fiber membrane, and cleaning the sodium citrate fiber membrane with ethanol to remove the redundant cation precursor. Then the crosslinked sodium citrate fiber membrane is placed in a drying oven at 60 ℃ for drying for standby.
(3) The anion and cation precursors react at the solid-liquid interface to generate the quantum dots
2mmol of Se is dissolved in a mixed solution of 4mL of TOP and 10mL of ODE, and the uniform Se-TOP-ODE anion precursor is obtained by stirring and dissolving at room temperature. Placing the crosslinked sodium citrate fiber membrane obtained in the step (2) into a 50mL inclined three-neck flask in N2Heated to 140 ℃ under an atmosphere. Then injecting the Se-TOP-ODE anion precursor into an inclined three-neck flask for reaction, after the reaction is carried out for 20min, pouring out the solution, precipitating with ethyl acetate and ethanol, cleaning with chloroform and acetone, and centrifuging to obtain Cd1-xZnxAnd (4) S quantum dots.
In summary, the quantum dot and the preparation method thereof provided by the invention use the solid-state nanofiber as the microreactor, the reaction temperature is low, the quantum dot can rapidly nucleate and grow at a solid-liquid interface, and the size of the quantum dot can be adjusted by controlling the size of the solid-state fiber membrane or the reaction temperature. In addition, the solid-state nanofiber membrane used as the microreactor can be repeatedly utilized, so that the cost is greatly saved. In addition, the method is simple to operate, easy to repeat and can be used for preparing the oil-soluble quantum dots.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (5)
1. A preparation method of quantum dots is characterized by comprising the following steps: firstly, preparing a solid fiber membrane, then placing the prepared solid fiber membrane into a cation precursor solution for crosslinking, removing redundant cation precursors, and drying to obtain a crosslinked solid fiber membrane; then injecting an anion precursor into the crosslinked solid fiber membrane, wherein the anion precursor and the cation precursor react at a solid-liquid interface to obtain quantum dots; wherein the size of the solid fiber membrane is nano-scale or micron-scale;
the cation precursor solution is prepared by dissolving a cation precursor in a solvent;
the cation precursor is CdCl2、ZnCl2、Cd(NO3)2、Zn(NO3)2、Pb(NO3)2、Cd(Ac)2、Zn(Ac)2、Pb(Ac)2One or more of;
the anion precursor is one or more of S-ODE, S-TOP, S-TOPO, S-OA, S-OLA, S-TBP, S-DDA, Se-ODE, Se-TOP, Se-TOPO and Se-TBP;
the anion precursor is formed by dissolving S or Se powder in corresponding organic matters.
2. The method for preparing the quantum dot according to claim 1, wherein the solid fiber membrane is one of a sodium citrate fiber membrane, a potassium citrate fiber membrane, a sodium alginate fiber membrane, a potassium alginate fiber membrane, a calcium alginate fiber membrane, a silica fiber membrane, and a titanium dioxide fiber membrane.
3. The method for preparing quantum dots according to claim 1, wherein the solid-state fiber membrane is prepared by an electrospinning method.
4. The method for preparing the quantum dot according to claim 1, wherein the temperature of the reaction of the anionic precursor and the cationic precursor at the solid-liquid interface is 120-160 ℃.
5. The method according to claim 1, wherein the solvent of the cationic precursor solution is ethanol.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1986726A (en) * | 2005-12-20 | 2007-06-27 | 中国科学院兰州化学物理研究所 | Preparing process of CdS semiconduct quantum dot |
| CN105602544A (en) * | 2015-12-24 | 2016-05-25 | 北京北达聚邦科技有限公司 | Preparation method for converting aqueous phase quantum dots into oil phase quantum dots |
| CN106010511A (en) * | 2016-05-18 | 2016-10-12 | Tcl集团股份有限公司 | Method for removing residual cationic precursors from oil-soluble quantum dots |
| CN106398680A (en) * | 2016-08-30 | 2017-02-15 | Tcl集团股份有限公司 | Oil-soluble blue-light quantum dot and preparation method thereof |
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| CN102993221B (en) * | 2012-12-13 | 2015-04-22 | 江南大学 | Method for preparing nano-zeolite metal-organic framework compounds by microreactor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1986726A (en) * | 2005-12-20 | 2007-06-27 | 中国科学院兰州化学物理研究所 | Preparing process of CdS semiconduct quantum dot |
| CN105602544A (en) * | 2015-12-24 | 2016-05-25 | 北京北达聚邦科技有限公司 | Preparation method for converting aqueous phase quantum dots into oil phase quantum dots |
| CN106010511A (en) * | 2016-05-18 | 2016-10-12 | Tcl集团股份有限公司 | Method for removing residual cationic precursors from oil-soluble quantum dots |
| CN106398680A (en) * | 2016-08-30 | 2017-02-15 | Tcl集团股份有限公司 | Oil-soluble blue-light quantum dot and preparation method thereof |
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