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In-situ formed copper nano cluster of double-layer shell structure and preparation method and application of copper nano cluster

An in-situ generation and nano-cluster technology, applied in the field of nanometers, can solve the problems that are not suitable for long-term sensing and biological imaging, it is difficult to form a stable uniform dispersion system, and it is difficult to enter the biological system, so as to achieve the promotion of luminous brightness, Effects that enhance luminescence and stability, and improve luminous brightness

Active Publication Date: 2019-09-13
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These large-sized particles are difficult to form a stable uniform dispersion system in aqueous solution, and are not easy to enter biological systems, making them unsuitable for long-term sensing and bioimaging

Method used

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  • In-situ formed copper nano cluster of double-layer shell structure and preparation method and application of copper nano cluster
  • In-situ formed copper nano cluster of double-layer shell structure and preparation method and application of copper nano cluster
  • In-situ formed copper nano cluster of double-layer shell structure and preparation method and application of copper nano cluster

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 1. Synthesis of trimethoxysilane-protected copper nanoclusters

[0044] 10 mL of acetonitrile was strictly deoxygenated in a round bottom flask. Put 0.02g of Cu(NO3) 2 was dissolved in deoxyacetonitrile, and then 80.6 μL of 3-mercaptopropyltrimethoxysilane (MPTS, ) was added to the above solution with Cu 2+ The mass ratio of the substance to MPTS is 1:3. The solution was vigorously stirred at room temperature at 1000 rpm for 30 minutes to finally obtain a colorless and transparent solution. The prepared CuNCs solution was stored in a refrigerator under nitrogen protection.

[0045] 2. Preparation of silica-coated nano-copper clusters

[0046] Select N,N-dimethylformamide (DMF) or dimethyl sulfoxide (DMSO) as the solvent to prepare silica-coated copper nanoclusters by hydrolyzing trimethoxysilane ligands on the surface of copper nanoclusters. clusters. Taking DMF as an example, the basic steps are as follows: First, 10 mL of dry DMF was mixed with 1 mL of trimethoxys...

Embodiment 2

[0062] 1. Synthesis of triethoxysilane-protected copper nanoclusters

[0063] 10 mL of acetonitrile was first strictly deoxygenated in a round bottom flask. 0.02gCu(NO 3 ) 2 Dissolve in deoxygenated acetonitrile, then add 62 μL (3-mercaptopropyl)triethoxysilane (MPTTS,) to the above solution, where Cu 2+ The amount ratio of the substance to MPTTS is 1:3. The solution was vigorously stirred at room temperature at a rotational speed of 1000 rpm for 30 minutes, and finally a colorless transparent solution was obtained. The prepared CuNCs solution was stored in a refrigerator under nitrogen protection.

[0064] 2. Preparation of silica-coated nano-copper clusters

[0065] DMF or DMSO was selected as the solvent to prepare silica-coated copper nanoclusters by hydrolyzing triethoxysilane ligands on the surface of copper nanoclusters. Taking DMSO as an example, the basic steps are as follows: First, 10 mL of dry DMSO was mixed with 1 mL of triethoxysilane-protected copper nanoc...

Embodiment 3

[0068] 1. Synthesis of mercaptosilane ligands

[0069] Glycol dimercaptoacetate (GDMA) and 3-(triethoxysilyl)propyl isocyanate (ICPTES) were used to prepare ligands for the synthesis of gold nanoclusters. Add a certain amount of GDMA (61.9 μL) and ICPTES (95.7 μL) to 20 mL of anhydrous acetonitrile, the ratio of the amount of the reaction substance is 1:1, and stir and heat at 70 ° C for 1 h. After the reaction was completed, a solution of a functionalized ligand (GDMA-ICPTES) containing a mercapto group at one end and a silane at the other end was obtained (the concentration of the substance was 19.17 mM). The obtained ligand solution was sealed and stored at low temperature.

[0070] 2. Preparation of nano-copper clusters stabilized by mercaptosilane

[0071] 10 mL of acetonitrile was first strictly deoxygenated in a round bottom flask. 0.0217g of Cu(NO 3 ) 2 Dissolve in deoxygenated acetonitrile, then add 2.016mL GDMA-ICPTES solution (n=19.17mM) to the above solution, ...

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Abstract

The invention discloses an in-situ formed copper nano cluster of a double-layer shell structure and a preparation method of the copper nano cluster. The preparation method comprises the steps: synthesizing a mercaptosilane ligand-protected copper nano cluster, preparing a silica-coated copper nano cluster, adding 3-thiopropyltrimethoxysilane or 3-aminopropyltrimethoxysilane to a DMF or DMSO solution of the copper nano cluster so as to obtain a mixture 3, stirring the mixture 3 vigorously, adding distilled water to the mixture 3, and performing stirring so as to prepare the mercapto-functionalized or amino-functionalized silica-coated copper nano cluster. The silica-coated copper nano cluster is obtained in a mode of in-situ formation of a silica shell, the surface is functionalized so as to form a double-layer structure, the luminance of the copper nano cluster is improved effectively, and the stability of the copper nano cluster is improved; and the invention also discloses a nano probe and a preparation method of the nano probe, and the nano probe is applied to detection of hydrogen sulfide.

Description

technical field [0001] The invention relates to the field of nanotechnology, in particular to a copper nano-cluster with an in-situ generated silica shell structure and a preparation method and application thereof. Background technique [0002] Luminescent metal nanoclusters have attracted extensive attention due to their special molecular structure, good biocompatibility, and excellent photoluminescence properties. Compared with gold and silver nanoclusters, copper nanoclusters have significant advantages in terms of facile synthesis and low cost, in addition to their multicolor emission. In recent years, scientists have devoted extensive efforts to research on the synthesis methods and potential uses of copper nanoclusters. Among them, thiol-protected copper nanoclusters (CuNCs) exhibit a unique aggregation-induced emission (AIE) phenomenon, which has aroused widespread interest among scientists. Its long lifetime (microscale), red / near-infrared emission, and its unique ...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/59G01N21/64B82Y30/00B82Y40/00
CPCC09K11/02C09K11/592C09K11/0883G01N21/643B82Y30/00B82Y40/00
Inventor 钱兆生丰慧敖航
Owner ZHEJIANG NORMAL UNIVERSITY
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