WO2020134141A1 - 一种量子点的制备方法 - Google Patents

一种量子点的制备方法 Download PDF

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WO2020134141A1
WO2020134141A1 PCT/CN2019/103207 CN2019103207W WO2020134141A1 WO 2020134141 A1 WO2020134141 A1 WO 2020134141A1 CN 2019103207 W CN2019103207 W CN 2019103207W WO 2020134141 A1 WO2020134141 A1 WO 2020134141A1
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quantum dot
precursor
trialkylamine
cationic precursor
quantum dots
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程陆玲
杨一行
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TCL Technology Group Co Ltd
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    • C09K11/881—Chalcogenides
    • C09K11/883—Chalcogenides with zinc or cadmium
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C09K11/00—Luminescent materials, e.g. electroluminescent or chemiluminescent
    • C09K11/08—Luminescent materials, e.g. electroluminescent or chemiluminescent containing inorganic luminescent materials
    • C09K11/62—Luminescent materials, e.g. electroluminescent or chemiluminescent containing inorganic luminescent materials containing gallium, indium or thallium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K11/00—Luminescent materials, e.g. electroluminescent or chemiluminescent
    • C09K11/08—Luminescent materials, e.g. electroluminescent or chemiluminescent containing inorganic luminescent materials
    • C09K11/88—Luminescent materials, e.g. electroluminescent or chemiluminescent containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements

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  • the present disclosure relates to the field of quantum dots, and in particular to a method for preparing quantum dots.
  • Nanomaterials are hailed as the most promising materials in the 21st century. Quantum dots have an important application and research value as an important branch of the field of nanomaterials.
  • quantum dots because of their special optical and electrical properties, they can be used in many fields such as light-emitting diodes, solar cells, fluorescent biomarkers, and lighting.
  • the preparation of the quantum dot material itself will involve the growth of the core and shell, where the growth of the shell layer has a greater impact on the photoelectric properties of the quantum dot, and for the quantum dot alloyed shell layer, it will involve the rate between different precursors Competition, the competition of this rate mainly depends on the concentration ratio of different precursors to adjust. However, this concentration-based adjustment of the reaction rate between different precursors will not only cause unnecessary waste of raw materials, but also cause defects such as lattice mismatch on the surface of the quantum dot shell.
  • the purpose of the present disclosure is to provide a method for preparing quantum dots, aiming to solve the problem that the prior art is likely to cause waste of raw materials and the existence of the surface of the generated quantum dot shell during the process of preparing quantum dot shell The problem of lattice mismatch.
  • a method for preparing quantum dots which includes the steps of:
  • the cationic precursor complex, the anionic precursor and the quantum dot core are mixed, and shell growth is performed on the surface of the quantum dot core to prepare the quantum dot.
  • the present disclosure provides a method for preparing quantum dots.
  • a cationic precursor complex is prepared, and then the The cationic precursor complex, the anionic precursor and the quantum dot core are mixed in an organic solvent, and the cationic precursor complex and the anionic precursor are reacted on the surface of the quantum dot core to form a quantum dot shell, thereby preparing the Quantum dots.
  • the covalent binding energy of the metal atom and the organic acid is reduced, thereby reducing the pyrolysis energy of the cationic precursor, that is, improving the cationic precursor
  • the activation energy of the body therefore, when the cationic precursor complex after the activation energy is increased and the anion precursor react to form a quantum dot shell, the growth temperature of the quantum dot shell can be effectively reduced and the quantum dot shell can be improved Lattice defects and lattice mismatch can also effectively reduce the use of cationic precursor materials.
  • FIG. 1 is a flowchart of a preferred embodiment of a method for preparing quantum dots disclosed in the present disclosure.
  • the present disclosure provides a method for preparing quantum dots. To make the objectives, technical solutions, and effects of the present disclosure clearer and more specific, the present disclosure will be described in further detail below. It should be understood that the specific embodiments described herein are only used to explain the present disclosure and are not intended to limit the present disclosure.
  • the present disclosure provides a flow chart of a preferred embodiment of a method for preparing quantum dots. As shown in the figure, the method includes the following steps:
  • the method for preparing quantum dots provided in this embodiment can effectively reduce the lattice defects and lattice mismatch of the quantum dot shell, and reduce the raw material cost.
  • the mechanism for achieving the above effect is as follows:
  • the charge balance of the cation changes due to the presence of the dipolar charge effect, resulting in a reduction in the covalent binding energy of the metal atom and the organic acid, thereby reducing the cationic precursor’s Pyrolysis energy, that is, the activation energy of the cationic precursor is improved; therefore, when the cationic precursor complex and the anionic precursor after the activation energy are mixed and reacted to form a quantum dot shell, the quantum dot shell can be effectively reduced Growth temperature and improve the lattice defects and lattice mismatch of the quantum dot shell, at the same time, it can also effectively reduce the use of cationic precursor materials.
  • the cationic precursor and the trialkylamine are mixed under the condition of 40-250° C. to combine the cationic precursor and the trialkylamine to prepare a cationic precursor complex. In some embodiments, the cationic precursor and the trialkylamine are mixed under an inert atmosphere for 10-60 minutes to combine the cationic precursor with the trialkylamine to prepare a cationic precursor complex.
  • the cationic precursor and the trialkylamine are mixed according to the molar ratio of the cationic precursor and the trialkylamine to be 1:1 to combine the cationic precursor and the trialkylamine to prepare Cationic precursor complex.
  • the cationic precursor is selected from one or more of zinc oleate, cadmium oleate, lead oleate, indium oleate, and copper oleate, but is not limited thereto.
  • the trialkylamine is selected from one or more of trioctylamine, triheptylamine, trihexylamine, tripentylamine, tributylamine, and tripropylamine, but is not limited thereto.
  • the trialkylamine is trioctylamine, and the trioctylamine is more non-polar and has a higher boiling point, which is more suitable for the synthesis of quantum dot shells in different temperature ranges .
  • the cationic precursor complex, the anionic precursor and the quantum dot core are mixed at 100-300°C, so that the cationic precursor complex and the anionic precursor are on the surface of the quantum dot core
  • the reaction generates a quantum dot shell to prepare the quantum dot.
  • the growth temperature of the shell layer and the concentration of the cation precursor are usually used to reduce the lattice defects and lattice loss during the growth process of the quantum dot shell layer; in this embodiment, due to the cation
  • a cationic precursor complex with stronger activation energy is generated, and the cationic precursor complex with the enhanced activation energy is mixed with an anionic precursor to form a quantum dot shell.
  • the growth temperature of the quantum dot shell layer can be effectively reduced and the lattice defects and lattice mismatch of the quantum dot shell layer can be improved.
  • the material of the cationic precursor can also be effectively reduced.
  • the cationic precursor complex and the quantum dot core are mixed in an organic solvent and heated to 100-300°C, and then an appropriate dropping rate is applied to the cationic precursor complex
  • An anion precursor is injected into the mixed solution with the quantum dot core, and the cationic precursor complex and the anion precursor are reacted on the surface of the quantum dot core to generate a quantum dot shell, thereby preparing the quantum dot.
  • the cationic precursor complex, the anionic precursor, and the quantum dot core are mixed at a molar mass ratio of the cationic precursor complex to the quantum dot core of 0.5-10 mmol: 100 mg.
  • the cationic precursor complex, the anionic precursor, and the quantum dot core are mixed at a molar mass ratio of the anionic precursor to the quantum dot core of 0.5-10 mmol: 100 mg.
  • the anionic precursor is selected from S-ODE, S-TOP, S-OA, Se-TOP, S-OLA, S-TBP, Se-TBP, Te-ODE, Te-OA, Te -One or more of TOP and Te-TBP, but not limited thereto.
  • the organic solvent is selected from one or more of octadecene, diphenyl ether, and paraffin oil, but is not limited thereto.
  • the quantum dot core is selected from one or more of binary phase quantum dots, ternary phase quantum dots, and quaternary phase quantum dots, but is not limited thereto.
  • the binary phase quantum dots include CdS, CdSe, CdTe, InP, AgS, PbS, PbSe, HgS, etc., but not limited thereto;
  • the ternary phase quantum dots include ZnCdS, CuInS, ZnCdSe, ZnSeS, ZnCdTe , PbSeS, etc., but not limited thereto;
  • the quaternary phase quantum dots include ZnCdS/ZnSe, CuInS/ZnS, ZnCdSe/ZnS, CuInSeS, ZnCdTe/ZnS, PbSeS/ZnS, etc., but are not limited thereto.
  • a preparation method of CdSe/ZnS core-shell quantum dots includes steps:
  • CdSe/ZnS core-shell quantum dots disperse 10 mmol of S in 5 ml of TOP at 80°C to dissolve and disperse it, and then cool to room temperature to prepare an S-TOP (anionic precursor) solution; take 100 mg of CdSe
  • S-TOP anionic precursor
  • the quantum dot core is dispersed into a three-necked flask containing 10ml of ODE for inert gas exhaust, and then 5ml of the zinc ion precursor complex solution in 1) is added to the CdSe quantum dot core solution, and then the temperature of the solution is increased
  • 3ml of S-TOP solution was gradually added dropwise to the CdSe quantum dot core solution containing zinc ion precursor complex for ZnS shell growth, and finally a certain thickness of CdSe/ZnS core-shell quantum was grown. point.
  • a preparation method of CdSe/InSe core-shell quantum dots includes steps:
  • CdSe/InSe core-shell quantum dots disperse 10 mmol of Se in 5 ml of TBP at 80° C. to dissolve and disperse it, and then cool to room temperature to prepare a Se-TBP (anionic precursor) solution; take 100 mg of CdSe
  • the quantum dot core is dispersed into a three-necked flask containing 10ml of ODE for inert gas exhaust, and then 5ml of the indium ion precursor complex solution in 1) is added to the CdSe quantum dot core solution, and then the temperature of the solution is increased
  • 3ml of Se-TBP solution was gradually added dropwise to the CdSe quantum dot core solution containing indium ion precursor complex for InSe shell growth, and finally a certain thickness of CdSe/InSe core-shell quantum was grown point.
  • a preparation method of CdSe/PbTe core-shell quantum dots includes steps:
  • Preparation of cationic precursor complex Take 8mmol of lead acetate, 4ml of OA, 8ml of ODE and add them to a three-necked flask. After heating at 200°C for 30 minutes, the temperature of the solution is reduced to 150°C, and then the zinc oleate solution Add 3ml of tripropylamine to maintain 200 °C heating and stirring for 20min, and then maintain to 100 °C, to prepare lead ion precursor complex solution;
  • CdSe/PbTe core-shell quantum dots Disperse 10 mmol of Te in 5 ml of TOP at 80°C to dissolve and disperse it, then cool to room temperature to prepare a Te-TOP (anionic precursor) solution; take 100 mg of CdSe
  • Te-TOP anionic precursor
  • the quantum dot core was dispersed into a three-necked flask containing 10ml of ODE for inert gas exhaust, and then 5ml of the lead ion precursor complex solution in 1) was added to the CdSe quantum dot core solution, and then the temperature of the solution was increased
  • 3ml of Te-TOP solution was gradually added dropwise to the CdSe quantum dot core solution containing lead ion precursor complex for PbTe shell growth, and finally a certain thickness of CdSe/PbTe core-shell quantum was grown. point.
  • the present disclosure provides a method for preparing quantum dots, by mixing a cationic precursor with a trialkylamine in advance to combine the cationic precursor with a trialkylamine to prepare a cationic precursor complex, and then The cationic precursor complex, the anionic precursor and the quantum dot core are mixed in an organic solvent, and the cationic precursor complex and the anionic precursor are reacted on the surface of the quantum dot core to form a quantum dot shell layer to prepare The quantum dots.
  • the covalent binding energy of the metal atom and the organic acid is reduced, thereby reducing the pyrolysis energy of the cationic precursor, that is, improving the cationic precursor
  • the activation energy of the body therefore, when the cationic precursor complex after the activation energy is increased and the anion precursor react to form a quantum dot shell, the growth temperature of the quantum dot shell can be effectively reduced and the quantum dot shell can be improved Lattice defects and lattice mismatch can also effectively reduce the use of cationic precursor materials.

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Abstract

公开一种量子点的制备方法，将阳离子前驱体与三烷基胺混合，使阳离子前驱体与三烷基胺结合，制得阳离子前驱体络合物，将阳离子前驱体络合物、阴离子前驱体以及量子点核混合在有机溶剂中，使阳离子前驱体络合物和阴离子前驱体在量子点核表面反应生成量子点壳层，制得量子点。三烷基胺与阳离子前驱体结合后，由于偶极电荷效应的存在促使了金属原子与有机酸的共价结合能降低，减少了阳离子前驱体的热解能，提升了阳离子前驱体的活化能；所述活化能提升后的阳离子前驱体络合物在与阴离子前驱体反应生成量子点壳层时，可有效降低量子点壳层的生长温度并改善量子点壳层的晶格缺陷和晶格失配，同时还可有效减少阳离子前驱体的用料。

Description

一种量子点的制备方法 技术领域
本公开涉及量子点领域，尤其涉及一种量子点的制备方法。
背景技术
纳米材料被誉为21世纪最具有前途的材料，量子点作为纳米材料领域的一个重要分支也有很重要的应用和研究价值。
对于发光量子点而言，由于其具有较特殊的光学和电学性能而能够应用在发光二极管、太阳能电池、荧光生物标记以及照明等多个领域。
量子点材料本身的制备会涉及到核壳的生长，其中，壳层的生长对于量子点的光电特性影响较大，对于量子点合金化壳层而言，会涉及到不同前驱体之间的速率竞争，该速率的竞争主要是依靠不同前驱物的浓度比例来调节。然而，这种依靠浓度来调节不同前驱体之间的反应速率不仅会造成不必要的原料浪费，而且也会使生成的量子点壳层表面存在晶格失配等缺陷。
因此，现有技术还有待于改进。
发明内容
鉴于上述现有技术的不足，本公开的目的在于提供一种量子点的制备方法，旨在解决现有技术在制备量子点壳层的过程中易造成原料浪费以及生成的量子点壳层表面存在晶格失配的问题。
本公开的技术方案如下：
一种量子点的制备方法，其中，包括步骤：
将阳离子前驱体和三烷基胺混合，使阳离子前驱体与三烷基胺之间结合，制得阳离子前驱体络合物；
将所述阳离子前驱体络合物、阴离子前驱体以及量子点核混合，在所述量子点核表 面进行壳层生长，制得所述量子点。
有益效果：本公开提供一种量子点的制备方法，通过预先将阳离子前驱体与三烷基胺混合，使阳离子前驱体与三烷基胺结合，制得阳离子前驱体络合物，然后将所述阳离子前驱体络合物、阴离子前驱体以及量子点核混合在有机溶剂中，使所述阳离子前驱体络合物和阴离子前驱体在量子点核表面反应生成量子点壳层，制得所述量子点。所述三烷基胺与阳离子前驱体结合后，由于偶极电荷效应的存在促使了金属原子与有机酸的共价结合能降低，从而减少了阳离子前驱体的热解能，即提升了阳离子前驱体的活化能；因此，将所述活化能提升后的阳离子前驱体络合物与阴离子前驱体反应生成量子点壳层时，可有效降低量子点壳层的生长温度并改善量子点壳层的晶格缺陷和晶格失配，同时还可有效减少阳离子前驱体的用料。
附图说明
图1为本公开一种量子点的制备方法较佳实施例的流程图。
具体实施方式
本公开提供一种量子点的制备方法，为使本公开的目的、技术方案及效果更加清楚、明确，以下对本公开进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本公开，并不用于限定本公开。
请参阅图1，本公开提供一种量子点的制备方法较佳实施例的流程图，其中，如图所示，包括步骤：
S100、将阳离子前驱体和三烷基胺混合，使阳离子前驱体与三烷基胺之间结合，制得阳离子前驱体络合物；
S200、将所述阳离子前驱体络合物、阴离子前驱体以及量子点核混合，在所述量子点核表面进行壳层生长，制得所述量子点。
本实施例提供的量子点制备方法能够有效降低量子点壳层的晶格缺陷以及晶格失配，并降低原料成本。实现上述效果的机理具体如下：
由于三烷基胺中的N原子中具有一对孤对电子，所述阳离子前驱体络合物的化学结构式为(R1) 3N：M(R2COO -)，其中，三个R1基团独立地选自碳原子数为2-10的烷基，R2为碳原子数为12-20的烷基，M为金属离子作为举例，当所述阳离子前驱体为油酸锌时，则其与三烷基胺形成的阳离子前驱体络合物的化学结构式为(R1) 3N：Zn(OA) 2。由于所述三烷基胺与阳离子前驱体结合后由于偶极电荷效应的存在使得阳离子所处的电荷平衡发生变化，导致金属原子与有机酸的共价结合能降低，从而减少了阳离子前驱体的热解能，即提升了阳离子前驱体的活化能；因此，将所述活化能提升后的阳离子前驱体络合物与阴离子前驱体混合反应生成量子点壳层时，可有效降低量子点壳层的生长温度并改善量子点壳层的晶格缺陷和晶格失配，同时还可有效减少阳离子前驱体的用料。
在一些实施方式中，将阳离子前驱体和三烷基胺在40-250℃的条件下混合，使阳离子前驱体与三烷基胺之间结合，制得阳离子前驱体络合物。在一些实施方式中，在惰性气氛条件下将所述阳离子前驱体和三烷基胺混合10-60min，使阳离子前驱体与三烷基胺结合，制得阳离子前驱体络合物。
在一些实施方式中，按照阳离子前驱体与三烷基胺的摩尔量比为1:1-2，将阳离子前驱体和三烷基胺混合，使阳离子前驱体与三烷基胺结合，制得阳离子前驱体络合物。
在一些实施方式中，所述阳离子前驱体选自油酸锌、油酸镉、油酸铅、油酸铟和油酸铜中的一种或多种，但不限于此。在一些实施方式中，所述三烷基胺选自三辛胺、三庚胺、三己胺、三戊胺、三丁胺和三丙胺中的一种或多种，但不限于此。
在一种具体的实施方式中，所述三烷基胺为三辛胺，所述三辛胺的非极性较强且具有较高的沸点，更加适合不同温度范围的量子点壳层的合成。
在一些实施方式中，将所述阳离子前驱体络合物、阴离子前驱体以及量子点核在100-300℃条件下混合，使所述阳离子前驱体络合物和阴离子前驱体在量子点核表面反应生成量子点壳层，制得所述量子点。现有技术在制备量子点壳层时通常会采用提高壳层生长温度和阳离子前驱体的浓度来降低量子点壳层生长过程中的晶格缺陷以及晶格缺失；而本实施方式中，由于阳离子前驱体经过所述三烷基胺的处理后生成了活化能更 强的阳离子前驱体络合物，将所述活化能提升后的阳离子前驱体络合物与阴离子前驱体混合反应生成量子点壳层时，可有效降低量子点壳层的生长温度并改善量子点壳层的晶格缺陷和晶格失配，同时还可有效减少阳离子前驱体的用料。
在一些具体的实施方式中，将所述阳离子前驱体络合物和量子点核混合在有机溶剂中并升温至100-300℃，然后采用适当的滴加速率向所述阳离子前驱体络合物和量子点核的混合溶液中注入阴离子前驱体，使所述阳离子前驱体络合物和阴离子前驱体在量子点核表面反应生成量子点壳层，制得所述量子点。
在一些实施方式中，按阳离子前驱体络合物与量子点核的摩尔质量比为0.5-10mmol：100mg，将所述阳离子前驱体络合物、阴离子前驱体以及量子点核混合。
在一些实施方式中，按阴离子前躯体与量子点核的摩尔质量比为0.5-10mmol：100mg，将所述阳离子前驱体络合物、阴离子前驱体以及量子点核混合。
在一些实施方式中，所述阴离子前驱体选自S-ODE、S-TOP、S-OA、Se-TOP、S-OLA、S-TBP、Se-TBP、Te-ODE、Te-OA、Te-TOP和Te-TBP中的一种或多种，但不限于此。在一些实施方式中，所述有机溶剂选自十八稀、二苯醚和石蜡油中的一种或多种，但不限于此。
在一些实施方式中，所述量子点核选自二元相量子点、三元相量子点和四元相量子点中的一种或多种，但不限于此。作为举例，所述二元相量子点包括CdS、CdSe、CdTe、InP、AgS、PbS、PbSe、HgS等，但不限于此；所述三元相量子点包括ZnCdS、CuInS、ZnCdSe、ZnSeS、ZnCdTe、PbSeS等，但不限于此；所述四元相量子点包括ZnCdS/ZnSe、CuInS/ZnS、ZnCdSe/ZnS、CuInSeS、ZnCdTe/ZnS、PbSeS/ZnS等，但不限于此。
下面通过具体实施例对本公开一种量子点固态膜的制备方法做进一步的解释说明：
实施例1
一种CdSe/ZnS核壳量子点的制备方法包括步骤：
1)、阳离子前驱体络合物的制备：取8mmol的醋酸锌、4ml OA、8ml ODE一起加入到三口烧瓶中，200℃加热排气30min后使溶液温度降低至150℃，然后向油酸锌溶液中加入3ml的三庚胺维持150℃加热搅拌30min，然后维持至100℃，制得锌离子前 驱体络合物溶液；
2)、CdSe/ZnS核壳量子点的制备：取10mmol的S分散到5ml的TOP中80℃使其溶解分散，然后冷却至室温制得S-TOP(阴离子前驱体)溶液；取100mg的CdSe量子点核分散到含有10ml的ODE的三口烧瓶中进行惰性气体排气，然后再取1)中锌离子前驱体络合物溶液5ml添加到含有CdSe量子点核溶液中，然后使溶液温度升高到250℃，再取3ml的S-TOP溶液逐步滴加道到含有锌离子前驱体络合物的CdSe量子点核溶液中进行ZnS壳层生长，最后得到生长一定厚度的CdSe/ZnS核壳量子点。
实施例2
一种CdSe/InSe核壳量子点的制备方法包括步骤：
1)、阳离子前驱体络合物的制备：取8mmol的醋酸铟、4ml OA、8ml ODE一起加入到三口烧瓶中，200℃加热排气30min后使溶液温度降低至150℃，然后向油酸锌溶液中加入3ml的三辛胺维持100℃加热搅拌50min，然后维持至100℃，制得铟离子前驱体络合物溶液；
2)、CdSe/InSe核壳量子点的制备：取10mmol的Se分散到5ml的TBP中80℃使其溶解分散，然后冷却至室温制得Se-TBP(阴离子前驱体)溶液；取100mg的CdSe量子点核分散到含有10ml的ODE的三口烧瓶中进行惰性气体排气，然后再取1)中铟离子前驱体络合物溶液5ml添加到含有CdSe量子点核溶液中，然后使溶液温度升高到200℃，再取3ml的Se-TBP溶液逐步滴加道到含有铟离子前驱体络合物的CdSe量子点核溶液中进行InSe壳层生长，最后得到生长一定厚度的CdSe/InSe核壳量子点。
实施例3
一种CdSe/PbTe核壳量子点的制备方法包括步骤：
1)、阳离子前驱体络合物的制备：取8mmol的醋酸铅、4ml OA、8ml ODE一起加入到三口烧瓶中，200℃加热排气30min后使溶液温度降低至150℃，然后向油酸锌溶液中加入3ml的三丙胺维持200℃加热搅拌20min，然后维持至100℃，制得铅离子前驱体络合物溶液；
2)、CdSe/PbTe核壳量子点的制备：取10mmol的Te分散到5ml的TOP中80℃使 其溶解分散，然后冷却至室温制得Te-TOP(阴离子前驱体)溶液；取100mg的CdSe量子点核分散到含有10ml的ODE的三口烧瓶中进行惰性气体排气，然后再取1)中铅离子前驱体络合物溶液5ml添加到含有CdSe量子点核溶液中，然后使溶液温度升高到300℃，再取3ml的Te-TOP溶液逐步滴加道到含有铅离子前驱体络合物的CdSe量子点核溶液中进行PbTe壳层生长，最后得到生长一定厚度的CdSe/PbTe核壳量子点。
综上所述，本公开提供一种量子点的制备方法，通过预先将阳离子前驱体与三烷基胺混合，使阳离子前驱体与三烷基胺结合，制得阳离子前驱体络合物，然后将所述阳离子前驱体络合物、阴离子前驱体以及量子点核混合在有机溶剂中，使所述阳离子前驱体络合物和阴离子前驱体在量子点核表面反应生成量子点壳层，制得所述量子点。所述三烷基胺与阳离子前驱体结合后，由于偶极电荷效应的存在促使了金属原子与有机酸的共价结合能降低，从而减少了阳离子前驱体的热解能，即提升了阳离子前驱体的活化能；因此，将所述活化能提升后的阳离子前驱体络合物与阴离子前驱体反应生成量子点壳层时，可有效降低量子点壳层的生长温度并改善量子点壳层的晶格缺陷和晶格失配，同时还可有效减少阳离子前驱体的用料。
应当理解的是，本公开的应用不限于上述的举例，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，所有这些改进和变换都应属于本公开所附权利要求的保护范围。

Claims (15)

  1. 一种量子点的制备方法，其特征在于，包括步骤：
    将阳离子前驱体和三烷基胺混合，使阳离子前驱体与三烷基胺之间结合，制得阳离子前驱体络合物；
    将所述阳离子前驱体络合物、阴离子前驱体以及量子点核混合，在所述量子点核表面进行壳层生长，制得所述量子点。
  2. 根据权利要求1所述量子点的制备方法，其特征在于，将阳离子前驱体和三烷基胺在40-250℃的条件下混合，使阳离子前驱体与三烷基胺发生结合，制得阳离子前驱体络合物。
  3. 根据权利要求1所述量子点的制备方法，其特征在于，在惰性气氛条件下将所述阳离子前驱体和三烷基胺混合10-60min，使阳离子前驱体与三烷基胺结合，制得阳离子前驱体络合物。
  4. 根据权利要求1所述量子点的制备方法，其特征在于，按照阳离子前驱体与三烷基胺的摩尔量比为1:1-2，将阳离子前驱体和三烷基胺混合，使阳离子前驱体与三烷基胺结合，制得阳离子前驱体络合物。
  5. 根据权利要求1-4任一所述量子点的制备方法，其特征在于，所述阳离子前驱体络合物的化学结构式为(R1) 3N：M(R2COO -)，其中，三个R1独立地选自碳原子数为2-10的烷基，R2为碳原子数为12-20的烷基，M为金属离子。
  6. 根据权利要求1所述量子点的制备方法，其特征在于，所述阳离子前驱体选自油酸锌、油酸镉、油酸铅、油酸铟和油酸铜中的一种或多种。
  7. 根据权利要求1所述量子点的制备方法，其特征在于，所述三烷基胺选自三辛胺、三庚胺、三己胺、三戊胺、三丁胺和三丙胺中的一种或多种。
  8. 根据权利要求6所述量子点的制备方法，其特征在于，所述三烷基胺为三辛胺。
  9. 根据权利要求1所述量子点的制备方法，其特征在于，将所述阳离子前驱体络合物、阴离子前驱体以及量子点核在100-300℃条件下混合，在所述量子点核表面进行壳层生长，制得所述量子点。
  10. 根据权利要求1所述量子点的制备方法，其特征在于，将所述阳离子前驱体络 合物和量子点核混合在有机溶剂中并升温至100-300℃，向所述阳离子前驱体络合物和量子点核的混合溶液中注入阴离子前驱体，使所述阳离子前驱体络合物和阴离子前驱体在量子点核表面反应生成量子点壳层，制得所述量子点。
  11. 根据权利要去10所述量子点的制备方法，其特征在于，所述有机溶剂选自十八稀、二苯醚和石蜡油中的一种或多种。
  12. 根据权利要求1所述量子点的制备方法，其特征在于，按阳离子前驱体络合物与量子点核的摩尔质量比为0.5-10mmol：100mg，将所述阳离子前驱体络合物、阴离子前驱体以及量子点核混合。
  13. 根据权利要求1所述量子点的制备方法，其特征在于，按阴离子前躯体与量子点核的摩尔质量比为0.5-10mmol：100mg，将所述阳离子前驱体络合物、阴离子前驱体以及量子点核混合。
  14. 根据权利要求1所述量子点的制备方法，其特征在于，所述阴离子前驱体选自S-ODE、S-TOP、S-OA、Se-TOP、S-OLA、S-TBP、Se-TBP、Te-ODE、Te-OA、Te-TOP和Te-TBP中的一种或多种。
  15. 根据权利要求1所述量子点的制备方法，其特征在于，所述量子点核选自二元相量子点、三元相量子点和四元相量子点中的一种或多种。
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