Method for preparing CdSe and ZnSe quantum dot nanometer granules

A nanoparticle and quantum dot technology, which is applied in chemical instruments and methods, color-changing fluorescent materials, binary selenium/tellurium compounds, etc., can solve the problem that selenourea cannot be used in the preparation of fat-soluble quantum dots, restricting promotion and application research, and synthesis costs. High photochemical stability, excellent spectral performance, and uniform size

Inactive Publication Date: 2008-12-31
HUNAN UNIV
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Problems solved by technology

The conventional method for preparing quantum dot nanoparticles is to use MO, M(Ac) 2 Metal substances such as (M=Cd, Zn) and trioctylphosphine oxide (TOP) are raw materials to prepare quantum dots (J.Am.Chem.Soc., 2001, 123 (36): 8844-8850; Nano.Lett., 2001, 1 (6): 333-337), adopt the above method to prepare quantum dots, the obtained product has excellent spectral performance, good monodispersity, strong photochemical stability, yet, TOP is bad as raw material stability, and the price Higher, the relative dosage is relatively large, making the synthesis cost high, which limits further promotion and application research
Pan proposed to use selenourea as a precursor substance (Adv.Mater., 2007, 17 (2): 176-179), but selenourea cannot be applied to the preparation of fat-soluble quantum dots
Deng and Jasieniak directly heat the aliphatic hydrocarbon mixture containing selenium powder (J.Phys.Chem.B, 2005, 109:16671-16675; J.Phys.Chem.B, 2005, 109:20665-20668), high temperature preparation of selenium precursor, but in this method, selenium is in the form of polymer isomers, which has disadvantages such as low solubility

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  • Method for preparing CdSe and ZnSe quantum dot nanometer granules
  • Method for preparing CdSe and ZnSe quantum dot nanometer granules
  • Method for preparing CdSe and ZnSe quantum dot nanometer granules

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Experimental program
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Effect test

Embodiment 1

[0030] The NaOH solution, sulfuric acid solution and oleylamine used in the experiment were deoxygenated by passing nitrogen gas for 20 minutes in advance. Such as figure 1 Build the experimental device shown in A, and add 33.2mg of selenium powder, 20mg of aluminum powder and 1mL of 2M NaOH solution to the three-necked flask in sequence under the protection of nitrogen. After 1 min, 2 mL of 2M sulfuric acid solution was injected. The generated gas was taken out under the action of nitrogen flow and introduced into 2 mL oleylamine to obtain oleylamine-hydrogen selenide complex. In another three-necked flask, heat 38.4mg CdO, 0.34g stearic acid and 4mL octadecene to 200°C to obtain a clear cadmium stearate solution, add 2mL oleylamine and 3g octadecylamine to the solution , continue to heat up to 240°C, stop heating, and inject the oleylamine-hydrogen selenide complex prepared above. After adding the precursor of selenium, keep the system temperature at 220°C, and take sampl...

Embodiment 2

[0033]The NaOH solution, sulfuric acid solution and oleylamine used were passed through nitrogen to deoxygenate for 20 minutes in advance. Under nitrogen protection, 30.0 mg of selenium powder, 18 mg of aluminum powder and 1 mL of 2M NaOH solution were sequentially added into the three-necked flask. After 1 min, 2 mL of 2M sulfuric acid solution was injected. The generated gas was taken out under the action of nitrogen flow and introduced into 2 mL oleylamine to obtain oleylamine-hydrogen selenide complex. In another three-necked flask, 24.3mg ZnO, 0.34g stearic acid and 4mL octadecene were slowly heated to 300°C to obtain a clear zinc stearate solution, and 2mL oleylamine and 3g octadecylamine were added to the solution . Continue to heat up to 320° C., stop heating, and inject the oleylamine-hydrogen selenide complex prepared above into the zinc stearate solution. After the precursor of selenium is added, the temperature of the system is maintained at 300°C, and samples a...

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Abstract

The invention discloses a method for preparing CdSe and ZnSe quantum dots nanometer particles. Aluminum powder and strong base solution are adopted for the reduction of selenium powder and sulphuric acid is added to generate hydrogen selenide, the hydrogen selenide is brought out by the flow of high purity nitrogen and dissolved in oil amine to obtain oil amine-hydrogen selenide composite; the oil amine-hydrogen selenide composite which is taken as a new selenium precursor, together with cadmium stearate and orzinc stearate, is used for preparing the CdSe and ZnSe quantum dots nanometer particles at high temperature; the prepared quantum dots nanometer particles have controllable spectrum and excellent performance and can be applied to the fields such as biological fluorescence label, optoelectronic materials, etc. Furthermore, the method for preparing quantum dots nanometer particles can avoid the adoption of trioctylphosphineoxide (TOP) which has strong toxicity and high price, and is low in cost and suitable for industrial production.

Description

technical field [0001] The invention relates to the preparation of nanometer materials, in particular to the preparation of fat-soluble CdSe and ZnSe quantum dot nanoparticles. Background technique [0002] Quantum Dots (QDs), also known as Semiconductor Nanocrystals, are nanocrystals composed of II-VI or III-V elements with a size of 1 to 20 nm. Quantum dots have molar The absorption coefficient is large, the excitation wavelength is wide and continuous, the emission wavelength is narrow and symmetrical, the Stokes shift is large, the fluorescence lifetime is long, and it is not easy to photobleach, and its fluorescence spectrum changes with the size and shape of quantum dots. Therefore, in Quantum dots have potential advantages in biomarkers, light-emitting diodes, lasers, solar cells and other optoelectronic devices and information storage applications, especially type II-VI quantum dots, which have been widely used in research and application because of their superior sp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04C09K9/00
Inventor 王柯敏刘剑波羊小海张鹏飞
Owner HUNAN UNIV
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