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Atom-precise silver nanoclusters with near-infrared electrochemiluminescence and its preparation method and application

A silver nanocluster, electrochemical technology, applied in the nano field, can solve the problems of instability of atomic number-accurate Au nanoclusters, limited application, and no atomic-accurate Ag nanocluster ECL, etc. The effect of chemical selectivity and anti-interference performance, wide application range and low cost

Active Publication Date: 2022-06-24
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the instability of the atomic number-precise Au nanoclusters used in the aqueous phase, the related ECL process is usually realized in the organic phase, which limits its further application.
[0004] At present, there is no practical technology and report on the realization and application of atomic number-accurate Ag nanocluster ECL process

Method used

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  • Atom-precise silver nanoclusters with near-infrared electrochemiluminescence and its preparation method and application
  • Atom-precise silver nanoclusters with near-infrared electrochemiluminescence and its preparation method and application
  • Atom-precise silver nanoclusters with near-infrared electrochemiluminescence and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] A method for regulating the electrochemical and electrochemiluminescence process of silver nanoclusters, the steps are as follows:

[0062] (1) Weigh 0.02g silver nitrate, add 5mL methanol solution;

[0063] (2) 9mL dichloromethane solution was added to step (1), stirred for 5min;

[0064] (3) 13.5 μL of 1,3-benzenedithiol solution was added to step (2), and stirred for 5min;

[0065] (4) in step (3), add 0.2g triphenylphosphine, add in the form of the dichloromethane solution of triphenylphosphine;

[0066] (5) 0.011 g of sodium borohydride was added to step (4), and added in the form of an aqueous sodium borohydride solution; the reaction was stirred at room temperature for 3h;

[0067] (6) after the reaction is completed, the Ag obtained in step (5) is 29 (BDT) 12 (TPP) 4 The nanocluster solution was mixed with methanol, centrifuged, purified three times, the supernatant was discarded, and the precipitate was dissolved in N,N-dimethylformamide to obtain Ag 29 (...

Embodiment 2

[0077] Step is with embodiment 1, difference is that in step (7) will purify good Ag 29 (BDT) 12 (TPP) 4 The nanoclusters were diluted to a monodisperse solution of 0.05 mg / mL, and 5 μL was drop-coated on the bare glassy carbon electrode. The uncoated bare glassy carbon electrode was used as a blank sample, and the dried electrode was placed in 4 mL of nitrogen-saturated 0.1 In M phosphate buffer solution, the differential pulse voltammetry curve of the cathode was tested under the condition of 800V high voltage, 3-level amplification.

[0078] The cathode differential pulse voltammetry curve of the blank sample obtained in this example Figure 8 shown, by Figure 8 It can be seen that the blank obtained in Example 2 has no obvious reduction potential.

[0079] Ag obtained in this example 29 (BDT) 12 (TPP) 4 Cathodic Differential Pulse Voltammetry of Nanoclusters Figure 9 shown, by Figure 9 It can be seen that the Ag obtained in Example 2 29 (BDT) 12 (TPP) 4 The ...

Embodiment 3

[0081] Step is with embodiment 1, difference is that in step (7) will purify good Ag 29 (BDT) 12 (TPP) 4 The nanoclusters were diluted to a monodisperse solution of 0.05 mg / mL, and 5 μL was drop-coated on the bare glassy carbon electrode. The uncoated bare glassy carbon electrode was used as a blank sample, and the dried electrode was placed in 4 mL of 0.1 M phosphate. In the buffer solution, the differential pulse voltammetry curve of the anode was tested under the condition of 800V high voltage and 3-level amplification.

[0082] The anode differential pulse voltammetry curve of the blank sample obtained in this example Figure 10 shown, by Figure 10 It can be seen that the blank obtained in Example 3 has no obvious oxidation potential.

[0083] Ag obtained in this example 29 (BDT) 12 (TPP) 4 Anodic Differential Pulse Voltammetry of Nanoclusters Figure 11 shown, by Figure 11 It can be seen that the Ag obtained in Example 2 29 (BDT) 12 (TPP) 4 The oxidation pot...

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Abstract

The invention belongs to the field of nanotechnology, and relates to a near-infrared electrochemiluminescent silver nano-cluster with precise atomic number and a preparation method and application thereof. Using silver nitrate as silver source, 1,3-benzenedithiol and triphenylphosphine as stabilizer, dichloromethane and methanol as solvent, N,N-dimethylformamide as dispersant, sodium borohydride as reducing agent Ag 29 (BDT) 12 (TPP) 4 nanoclusters. The invention is a one-pot synthesis method, the required raw materials are cheap and easy to obtain, the synthesis device is simple, the conditions are mild, and the operation is safe. The resulting Ag 29 (BDT) 12 (TPP) 4 Nanoclusters have good monodispersity and stability, and can produce tunable electrochemical and electrochemiluminescent processes.

Description

technical field [0001] The invention belongs to the field of nanotechnology, and relates to an atomic number-accurate silver nanocluster with near-infrared electrochemiluminescence and a preparation method and application thereof. Background technique [0002] Precise atomic number noble metal nanoclusters are composed of a certain number of central atoms and ligands, and have identifiable molecular structures and optical, electrical, physical and chemical properties (J.Am.Chem.Soc.2015,137,12906– 12913). Atomically precise noble metal nanoclusters with molecular size-limited noble metal atoms and discrete electronic energy levels have been used in catalysis (J.Am.Chem.Soc.2020,142,4141–4153), chemiluminescence (Angew.Chem. Int.Edit.2019,58,6276–6279), light energy conversion (Acc.Chem.Res.2016,49,1514–1523) and other fields show broad application prospects. [0003] Electrochemiluminescence (ECL), also known as electrochemiluminescence, is a process that generates highly ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/26G01N27/30G01N27/327G01N21/76
CPCG01N27/26G01N27/30G01N27/3278G01N21/76
Inventor 邹桂征高旭雯
Owner SHANDONG UNIV
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