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Preparation method and application of near-infrared IIb region metal ion (M/Zn, Mn) doped silver telluride quantum dots

A technology of metal ions and quantum dots, which is applied in the rapid synthesis of zinc or manganese-doped silver telluride quantum dots and the preparation field by hot injection method, can solve the problems of difficulty in meeting the requirements of high-resolution imaging, the decrease of fluorescence performance of quantum dots, and the problems of silver telluride quantum dots. Solubility product is small and other problems, to achieve the effect of good monodispersity, long wavelength, high signal ratio

Active Publication Date: 2022-04-12
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

(Appl. Nano Mater. 2020, 3, 6071., Nanoscale 2021, 13, 163.) There are some reports on the synthesis of silver telluride quantum dots, but the solubility product of silver telluride is small, the band gap is narrow, and the emission wavelength Sensitive to changes, there is a problem that the wavelength is difficult to adjust to the near-infrared IIb region, or the fluorescence quantum yield is low, and it is difficult to meet the requirements of high-resolution imaging in vivo
[0004]The fluorescence performance of quantum dots depends on the radiative recombination of excitons. And non-radiative recombination, defects inside or on the surface of quantum dots will cause non-radiative recombination of excitons, resulting in reduced fluorescence performance of quantum dots

Method used

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  • Preparation method and application of near-infrared IIb region metal ion (M/Zn, Mn) doped silver telluride quantum dots
  • Preparation method and application of near-infrared IIb region metal ion (M/Zn, Mn) doped silver telluride quantum dots
  • Preparation method and application of near-infrared IIb region metal ion (M/Zn, Mn) doped silver telluride quantum dots

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Experimental program
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Effect test

Embodiment 1

[0040] Preparation of zinc-doped silver telluride quantum dots:

[0041](1) Preparation of tellurium precursor: Weigh 29.7mg of tellurium powder and add it to a 25mL two-necked flask with a condenser tube, pass in argon for 10 minutes, add 2mL of tri-n-octylphosphine, pump for 15 minutes, and ventilate for 15 minutes , repeated three times, heated up to 150°C, stirred and dissolved into a clear light yellow solution, cooled to room temperature for later use.

[0042] (2) Weigh 21.7mg of silver acetate and 11.9mg of zinc acetate into a 50mL three-neck flask with a condenser tube, add 4.7mL of octadecene, pump for 15 minutes, pass argon for 15 minutes, and add 0.26mL of octyl mercaptan , evacuate for 15 minutes, pass argon for 15 minutes, repeat three times, stir and heat to 110°C, silver acetate dissolves, the solution becomes clear and light yellow, then rapidly heat to 170°C, and quickly inject 0.3mL tellurium precursor at 170°C, Rapidly cool down to 100°C and keep warm for ...

Embodiment 2

[0045] Preparation of manganese-doped silver telluride quantum dots:

[0046] (1) Preparation of tellurium precursor: Weigh 55.0 mg of tellurium powder and add it to a 25 mL two-necked flask with a condenser, pass argon for 10 minutes, add 3 mL of tri-n-octylphosphine, pump for 15 minutes, and ventilate for 15 minutes , repeated three times, heated up to 150°C, stirred and dissolved into a clear light yellow solution, cooled to room temperature for later use.

[0047] (2) Weigh 66.8mg of silver acetate and 10.6mg of manganese acetate into a 50mL three-neck flask with a condenser, add 8.5mL of octadecene, pump for 15 minutes, pass argon for 15 minutes, and add 0.52mL of octyl mercaptan , evacuate for 15 minutes, pass argon for 15 minutes, repeat three times, stir and heat to 110°C, silver acetate dissolves, the solution becomes clear and light yellow, then rapidly heat to 170°C, and quickly inject 1.0mL tellurium precursor at 170°C, React at 170-180 degrees Celsius for 5 minut...

Embodiment 3-5

[0050] The preparation method of embodiment 3-5 is the same as embodiment 1, wherein different raw materials, consumption and proportioning ratio are shown in the following table:

[0051] project Example 3 Example 4 Example 5 Silver source and dosage Silver acetate 33.4mg Silver acetate 21.7mg Silver nitrate 22mg Zinc source and dosage Zinc acetate 5.8mg Zinc acetate 17.4mg Zinc nitrate 24.6mg non-coordinating solvent Octadecene Octadecene liquid paraffin Thiol ligand Octylthiol dodecyl mercaptan Octylthiol Organic phosphine Trioctylphosphine Tributylphosphine Trioctylphosphine Tellurium powder dosage 29.7mg 29.7mg 36.8mg

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Abstract

The invention discloses a near-infrared IIb region metal ion (M = Zn, Mn) doped silver telluride quantum dot and a preparation method and application thereof. The synthesized quantum dot is excellent in fluorescence performance and can be used for fluorescence imaging in a near-infrared IIb region (1500-1700 nm), and the penetration depth and the spatial resolution of imaging are improved. The synthesis method mainly comprises the following steps: mixing and stirring a silver source, a zinc source or a manganese source and a sulfydryl ligand, introducing inert gas, and heating and dissolving to obtain a mixed solution of a silver precursor and a zinc or manganese precursor; and rapidly injecting a tellurium precursor at the temperature of 160-170 DEG C, and reacting for a period of time to obtain the zinc or manganese doped silver telluride quantum dot. The method is simple to operate, good in repeatability and relatively low in cost; the prepared zinc or manganese doped silver telluride quantum dot is uniform in particle size distribution, good in monodispersity and high in fluorescence quantum yield, and keeps good stability under the conditions of continuous laser irradiation, long-time storage, further ligand modification and the like. The method can be widely applied to the fields of fluorescence living body imaging, biomedical detection, photoelectric devices and the like.

Description

technical field [0001] The invention relates to the fields of nanometer material preparation and medical material science, in particular to a thermal injection method for rapidly synthesizing zinc or manganese doped silver telluride quantum dots, a preparation method and an application. Background technique [0002] In vivo imaging technology is widely used in clinical practice and biomedical research, among which non-invasive imaging methods mainly include computed tomography (CT), magnetic resonance imaging (MRI), ultrasound (US), positron emission tomography (PET) and Fluorescence imaging, etc., play an important role in the diagnosis, monitoring and prevention of some diseases. Fluorescence imaging has the characteristics of non-radiation and fast response, and has attracted more and more attention. However, biological substances such as water, hemoglobin, and melanin in living organisms and different biological tissues will produce photon absorption and scattering, and...

Claims

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Application Information

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IPC IPC(8): C09K11/88B82Y30/00B82Y20/00A61K49/00
Inventor 崔然周亦飞黄彪张明曦
Owner WUHAN UNIV
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