Near-infrared electrochemiluminescence atom precision type silver nanocluster and preparation method and application thereof
A silver nanocluster, chemiluminescence technology, applied in the nano field, can solve the problems such as no atomic precise Ag nanocluster ECL, limited application, and atomic precise Au nanocluster instability, etc. The effect of chemical selectivity and anti-interference performance, wide application range and low cost
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Embodiment 1
[0061] A method for regulating the electrochemistry and electrochemiluminescence process of silver nanoclusters, the steps are as follows:
[0062] (1) Take by weighing 0.02g silver nitrate, add 5mL methanol solution;
[0063] (2) Add 9 mL of dichloromethane solution to step (1), and stir for 5 min;
[0064] (3) Add 13.5 μL of 1,3-benzenedithiol solution to step (2), and stir for 5 minutes;
[0065] (4) Add 0.2g triphenylphosphine to step (3), add in the form of dichloromethane solution of triphenylphosphine;
[0066] (5) Add 0.011 g of sodium borohydride to step (4) in the form of an aqueous solution of sodium borohydride; stir and react at room temperature for 3 hours;
[0067] (6) After the reaction is completed, the Ag obtained in step (5) 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 (BDT) 12 (TPP) 4 A...
Embodiment 2
[0077] Step is the same as Example 1, and difference is that in step (7) the Ag that will be purified 29 (BDT) 12 (TPP) 4 Dilute the nanoclusters to a monodisperse solution of 0.05 mg / mL, take 5 μL drop-coated on the bare glassy carbon electrode, take the bare glassy carbon electrode that has not been drip-coated as a blank sample, and place the dried electrode 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 and three levels of amplification.
[0078] The cathode differential pulse voltammetry curve of the blank sample obtained in this embodiment Figure 8 shown by Figure 8 It can be seen that the blank sample obtained in Example 2 has no obvious reduction potential.
[0079] The Ag obtained in this embodiment 29 (BDT) 12 (TPP) 4 Cathode differential pulse voltammetry curves of nanoclusters Figure 9 shown by Figure 9 It can be seen that the ...
Embodiment 3
[0081] Step is the same as Example 1, and difference is that in step (7) the Ag that will be purified 29 (BDT) 12 (TPP) 4 Dilute the nanoclusters to a monodisperse solution of 0.05 mg / mL, take 5 μL drop-coated on the bare glassy carbon electrode, take the un-coated bare glassy carbon electrode as a blank sample, and place the dried electrode in 4 mL of 0.1M phosphate In the buffer solution, the differential pulse voltammetry curve of the anode was tested under the condition of 800V high voltage and three levels of amplification.
[0082] The anode differential pulse voltammetry curve of the blank sample obtained in this embodiment Figure 10 shown by Figure 10 It can be seen that the blank sample obtained in Example 3 has no obvious oxidation potential.
[0083] The Ag obtained in this embodiment 29 (BDT) 12 (TPP) 4 Anodic differential pulse voltammetry curves of nanoclusters Figure 11 shown by Figure 11 It can be seen that the Ag obtained in Example 2 29 (BDT) 1...
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