A double ruthenium metal complex and its application in near-infrared electrochromic thin films
A technology of metal complexes and complexes, applied in the direction of ruthenium organic compounds, color-changing fluorescent materials, platinum group organic compounds, etc., can solve the problems of tedious and time-consuming
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Embodiment 1
[0056] Embodiment 1, the synthesis of double ruthenium conjugated metal complexes (formula I)
[0057] 1) Preparation of 1,2,4,5-(2-pyridyl)benzene ligand (Formula III)
[0058] The synthesis of 1,2,4,5-(2-pyridyl)benzene ligand refers to Yao Chang-Jiang, Zhong Yu-Wu, YaoJiannian.Charge Delocalization in a Cyclometalated Bisruthenium ComplexBridged by a Noninnocent 1.2.4.5-Tetra(2- pyridyl) benzene Ligand, J. Am. Chem. Soc. 2011, 133, 15697-15706. The reaction equation is as follows:
[0059]
[0060] 2) Preparation of 4,4',4"-trysteryl terpyridine bis-ruthenium complex (Formula Ⅱ)
[0061] The reaction equation is as follows:
[0062]
[0063] Reflux the reaction flask containing trichloro-4,4',4"-trimethylcarbocarboxyterpyridine ruthenium(III) (37mg, 0.060mmol), silver trifluoromethanesulfonate (52mg, 0.20mmol), 40mL acetone solvent , filtered after reacting for 3h, and added 1,2,4,5-(2-pyridyl)benzene ligand (11.6mg, 0.03mmol), 10mL N,N-dimethylformamide, 10mL ter...
Embodiment 2
[0072] Embodiment 2, preparation of double ruthenium conjugated metal complex multilayer film
[0073] SnO was coated by scraping method 2 : Sb slurry was applied to the glass sheet based on FTO, after natural drying, it was placed in a muffle furnace, and the temperature was gradually raised to 450 ° C, calcined for 15 min, cooled to 80 ° C after the calcination, and immersed in 0.30 mM 4,4 Methanol (0.1M n Bu 4 NOH) solution, soaked at room temperature for 12h, then washed off the unadsorbed dye on the surface with methanol and acetone to obtain a monolayer film of double ruthenium conjugated metal complexes, and then alternately immersed in ZrOCl 2 Multilayer films with different layers can be obtained by complex assembly in aqueous solution and methanol solution of double ruthenium complexes.
[0074] The schematic diagram of the structure of the double ruthenium conjugated metal complex multilayer film prepared in this example is as follows figure 1 As shown, the stru...
Embodiment 3
[0076] Embodiment 3, the assembly of electrochromic device
[0077] according to Figure 4 The schematic diagram of the structure shown in the assembled electrochromic device:
[0078] Prepared with Example 2
[0079] FTO / SnO 2 :Sb / (1) n (Zr) n-1 (n=1, 2, 3 or 4) The thin film is used as the working electrode, the FTO glass is used as the counter electrode, the solvent is acetonitrile, and 0.1M tetra-n-butyl perchlorate ammonium is used as the electrolyte solution. The 200μm thick glass separates the working electrode and the counter electrode, so that there is a certain gap filled with electrolyte solution, and then encapsulated with epoxy resin. All tested electrochromic devices with an area of 1 x 1 cm 2 .
[0080] The electrochemical test of the electrochromic device thin film of above-mentioned preparation is as follows Figure 5 As shown in (a), it can be seen that the thin film FTO / SnO 2 : Sb / 1 has two reversible redox peaks at +0.36V and +0.73V (reference el...
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