A kind of preparation method of rare earth doped alkaline earth metal sulfide nanomaterial

An alkaline earth metal and nanomaterial technology, which is applied in chemical instruments and methods, luminescent materials, nanotechnology, etc., can solve the problems of failing to realize the size control of nanomaterials, affecting the synthesis of nanomaterials, and difficult to control the purity, and achieving easy amplification and synthesis. , uniform size and morphology, easy to control synthesis conditions

Active Publication Date: 2022-03-22
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, Meijerink et al. reported the use of diisopropyl dithiocarbamate metal salt as a precursor for synthesis. The synthesized nanoparticles are nearly spherical, about 10 nm, and have good dispersion. However, the precursor used in this synthesis method is two The metal salt of isopropyl dithiocarbamate cannot be purchased, and can only be synthesized by oneself, and the synthesis steps are cumbersome, the reaction takes a long time, and the purity is not easy to control, which will affect the synthesis of nanomaterials. Size regulation (AndriesMeijerink et al."Lanthanide-Doped CaS and SrS Luminescent Nanocrystals: ASingle-Source Precursor Approach for Doping", J.Am.Chem.Soc.2014,136,16533-16543)

Method used

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  • A kind of preparation method of rare earth doped alkaline earth metal sulfide nanomaterial
  • A kind of preparation method of rare earth doped alkaline earth metal sulfide nanomaterial
  • A kind of preparation method of rare earth doped alkaline earth metal sulfide nanomaterial

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Example 1: CaS of different sizes: 0.07mol% Ce 3+ Preparation of nanoparticles

[0065] Weigh 0.9993mmol Ca(CH 3 COO) 2 ·H 2 O, 0.0007mmol Ce(CH 3 COO) 3 4H 2 O, then add 4mL oleic acid, 8mL oleylamine and 8mL trioctylamine, heat to 120°C with nitrogen gas and keep warm for 30 minutes to form a transparent solution A, then lower to room temperature; weigh 3mmol of DPTU, dissolve in 10mL ethanol, Add it dropwise to solution A, continue to stir for 10 minutes to fully mix, heat up to 80°C, keep warm for 30 minutes, and form a transparent solution B; heat up to 320°C, keep warm for 1 hour, and drop to room temperature; add 20mL of ethanol to precipitate, separate and wash Several times, get about 15nm oil-soluble CaS:0.07mol%Ce 3+ Nanoparticles; at the same time, under the condition of other reaction conditions unchanged, changing the volume ratio of solvent oleic acid, oleylamine and trioctylamine to 2:3:5, 1:3:6, 1:6:3 can be synthesized accordingly Oil-soluble C...

Embodiment 2

[0066] Embodiment 2: CaS:0.07mol% Ce 3+ Preparation of @CaS single-layer core-shell nanoparticles

[0067] Weigh 0.9993mmol Ca(CH 3 COO) 2 ·H 2 O, 0.0007mmol Ce(CH 3 COO) 3 4H 2 O, then add 4mL oleic acid, 8mL oleylamine and 8mL trioctylamine, heat to 120°C with nitrogen gas and keep warm for 30 minutes to form a transparent solution A, then lower to room temperature; weigh 3mmol of DPTU, dissolve in 10mL ethanol, Add it dropwise to solution A, continue to stir for 10 minutes to fully mix, heat up to 80°C, keep warm for 30 minutes, and form a transparent solution B; heat up to 320°C, keep warm for 1 hour, and drop to room temperature; add 20mL of ethanol to precipitate, separate and wash Several times, get about 15nm oil-soluble CaS:0.07mol%Ce 3+ nanoparticles.

[0068] Oil-soluble CaS:0.07mol%Ce 3+ Nanoparticles are used as core seed crystals for core-shell coating. Weigh 1mmolCa(CH 3 COO) 2 ·H 2 O, then add 4mL oleic acid, 8mL oleylamine and 8mL trioctylamine, h...

Embodiment 3

[0069] Embodiment 3: CaS:0.07mol% Ce 3+Preparation of @CaS@CaS multi-shell core-shell nanoparticles

[0070] Weigh 0.9993mmol Ca(CH 3 COO) 2 ·H 2 O, 0.0007mmol Ce(CH 3 COO) 3 4H 2 O, then add 4mL oleic acid, 8mL oleylamine and 8mL trioctylamine, heat to 120°C with nitrogen gas and keep warm for 30 minutes to form a transparent solution A, then lower to room temperature; weigh 3mmol of DPTU, dissolve in 10mL ethanol, Add it dropwise to solution A, continue to stir for 10 minutes to fully mix, heat up to 80°C, keep warm for 30 minutes, and form a transparent solution B; heat up to 320°C, keep warm for 1 hour, and drop to room temperature; add 20mL of ethanol to precipitate, separate and wash Several times, get about 15nm oil-soluble CaS:0.07mol%Ce 3+ nanoparticles.

[0071] Oil-soluble CaS:0.07mol%Ce 3+ Nanoparticles are used as core seed crystals for core-shell coating. Weigh 1mmolCa(CH 3 COO) 2 ·H 2 O, then add 4mL oleic acid, 8mL oleylamine and 8mL trioctylamine,...

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Abstract

A preparation method of rare earth-doped alkaline earth metal sulfide nanomaterial MS:xmol%Ln, M in MS:xmol%Ln is selected from alkaline earth metals Ca, Sr or Ba; S represents sulfur; Ln represents lanthanide rare earth ions; xmol % represents the percentage of lanthanide rare earth ions in the total number of moles of alkaline earth metals and lanthanide rare earth ions, 0

Description

technical field [0001] The invention belongs to the technical field of nano-luminescent materials, and in particular relates to a preparation method of a rare-earth-doped alkaline-earth metal sulfide nano-material. Background technique [0002] In recent years, rare earth-doped inorganic nanoluminescent materials have received widespread attention. Due to their excellent performance, these materials are widely used in three-dimensional displays, anti-counterfeiting technology, solid-state lasers, optical storage, solar cells, biological detection, and imaging. At present, the research on rare earth doped inorganic nano-fluorescent materials mainly focuses on rare earth doped fluorides (such as NaYF 4 , NaGdF 4 , CaF 2 ) and other systems, there are few studies on rare earth doped alkaline earth metal sulfide (MS) (M=Ca, Sr, Ba) nanoluminescent materials. [0003] Rare earth doped alkaline earth metal sulfides have a cubic phase structure, the space point group is Fm-3m, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/56C09K11/02B82Y30/00B82Y40/00
CPCC09K11/7718C09K11/7731C09K11/7768C09K11/7786C09K11/02B82Y30/00B82Y40/00
Inventor 郑伟张美然陈学元高宇黄萍
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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