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Preparing method for Gd-Zn-Cu-In-S@ZnS core-shell quantum dot with adjustable emission wavelength

A technology of core-shell quantum dots and emission wavelengths, which is applied in chemical instruments and methods, luminescent materials, nanotechnology, etc., and can solve problems such as emission wavelengths not reaching the near-infrared region and the impact of fluorescence quantum yields.

Inactive Publication Date: 2016-10-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Recently, paramagnetic ions (such as Mn 2+ and Gd 3+ ) doped quantum dots to prepare dual-mode imaging probes have been reported. However, these doped quantum dots not only greatly affect the fluorescence quantum yield, but also the emission wavelength cannot reach the near-infrared region. Therefore, the preparation of near-infrared fluorescence / magnetic resonance Imaging dual-modal imaging probes without losing their quantum yield remains a formidable challenge

Method used

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  • Preparing method for Gd-Zn-Cu-In-S@ZnS core-shell quantum dot with adjustable emission wavelength
  • Preparing method for Gd-Zn-Cu-In-S@ZnS core-shell quantum dot with adjustable emission wavelength
  • Preparing method for Gd-Zn-Cu-In-S@ZnS core-shell quantum dot with adjustable emission wavelength

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Effect test

Embodiment 1

[0040] 1) 5mmol gadolinium chloride GdCl 3 .6H 2 0, 15mmol sodium oleate is dissolved in the mixture of 20mL ethanol and 60mL water, condenses and refluxes to form oleic acid gadolinium, the above-mentioned oleic acid gadolinium mixture is transferred in the separatory funnel, extracts the organic layer after adding normal hexane, and washes with pure water, in The solvent was removed on a rotary evaporator to obtain pure gadolinium oleate Gd(OA) 3 ;

[0041] 2) The above 0.4mmol gadolinium oleate Gd(OA) 3 , 0.1mmol copper oleate Cu(OA) 2 , 0.2mmol indium oleate In(OA) 3 , 0.1mmol zinc oleate Zn(OA) 2 Add oleic acid (OA) and octadecene (ODE) into a mixed solvent (volume ratio OA: ODE = 1:20), vacuumize for 30 minutes and heat to 120°C under the protection of argon. After the solution is clarified, inject 1 mL of double p-Chlorophenyltrichloroethane (DDT), the solution turns bright yellow, quickly inject the 0.3mmol sulfur powder mixture prepared in advance (the sulfur po...

Embodiment 2

[0045] 1) 5mmol gadolinium chloride GdCl 3 .6H 2 0, 15mmol sodium oleate is dissolved in the mixture of 20mL ethanol and 40mL water, condenses and refluxes to form oleic acid gadolinium, transfers the above-mentioned oleic acid gadolinium mixture in the separatory funnel, extracts the organic layer after adding normal hexane, and washes with pure water, in The solvent was removed on a rotary evaporator to obtain pure gadolinium oleate Gd(OA) 3 ;

[0046] 2) The above 0.2mmol gadolinium oleate Gd(OA) 3 , 0.1mmol copper oleate Cu(OA) 2 , 0.2mmol indium oleate In(OA) 3 , 0.2mmol zinc oleate Zn(OA) 2 Add it into a mixed solvent of oleic acid (OA) and octadecene (ODE) (volume ratio: OA: ODE = 1:15), vacuumize for 30 minutes and heat to 120°C under the protection of argon. After the solution is clarified, inject 1 mL of double p-Chlorophenyltrichloroethane (DDT), the solution turns bright yellow, quickly inject the 0.3mmol sulfur powder mixture prepared in advance (the sulfur ...

Embodiment 3

[0050] 1) 5mmol gadolinium chloride GdCl 3 .6H 2 0, 15mmol sodium oleate is dissolved in the mixture of 20mL ethanol and 50mL water, condenses and refluxes to form oleic acid gadolinium, transfers the above-mentioned oleic acid gadolinium mixture in the separatory funnel, extracts the organic layer after adding normal hexane, and washes with pure water, in The solvent was removed on a rotary evaporator to obtain pure gadolinium oleate Gd(OA) 3 ;

[0051] 2) The above 0.6mmol gadolinium oleate Gd(OA) 3 , 0.1mmol copper oleate Cu(OA) 2 , 0.2mmol indium oleate In(OA) 3 , 0.3mmol zinc oleate Zn(OA) 2 Add it into a mixed solvent of oleic acid (OA) and octadecene (ODE) (volume ratio: OA: ODE = 1:10), vacuumize for 30 minutes and heat to 120°C under the protection of argon. After the solution is clarified, inject 1 mL of double p-Chlorophenyltrichloroethane (DDT), the solution turns bright yellow, quickly inject the 0.3mmol sulfur powder mixture prepared in advance (the sulfur ...

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Abstract

The invention relates to a preparation method of Gd–Zn–Cu–In–S@ZnS core-shell quantum dots with adjustable emission wavelength; Gd–Zn–Cu–In–S@ZnS core-shell quantum dots were synthesized by high-temperature oil-phase synthesis to prepare near-infrared fluorescence and magnetic resonance imaging dual-modal probes for in vivo diagnostics. The characteristics of the present invention are: the combination of fluorescence imaging and magnetic resonance imaging greatly improves the sensitivity of diagnosis; the Gd–Zn–Cu–In–S@ZnS core-shell quantum dots can be made by adjusting the Zn / Cu molar ratio The emission wavelength is controlled at 570-735nm; Gd 3+ The introduction of Gd–Zn–Cu–In–S@ZnS core-shell quantum dots has little effect on the quantum yield, and the quantum yield is as high as about 40%.

Description

technical field [0001] The invention relates to the technical field of preparation of compound semiconductor nanomaterials, and more specifically relates to a preparation method of Gd-Zn-Cu-In-S@ZnS core-shell quantum dots with adjustable emission wavelength. Background technique [0002] In recent years, the combination of magnetic resonance imaging, which provides anatomical details and high-quality soft-tissue 3-D information in a noninvasive manner, and optical imaging, which has relatively better detection sensitivity, has gained intense attention However, the tissue penetration depth is limited, so magnetic resonance / fluorescence MRI / fluorescence dual-modal imaging will have broad application prospects. During surgery, magnetic resonance / fluorescence dual-modality imaging can determine the site of surgical resection by fluorescence imaging, and ensure that the tumor tissue is completely removed by magnetic resonance imaging. Therefore, magnetic resonance / fluorescence d...

Claims

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Application Information

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IPC IPC(8): C09K11/84B82Y20/00B82Y40/00
CPCC09K11/7702B82Y20/00B82Y40/00
Inventor 常津武玉东郭伟圣宫晓群
Owner TIANJIN UNIV
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