A single-layer electrochromic device and its preparation method
A technology of color-changing devices and electrochromic materials, which can be used in instruments, nonlinear optics, optics, etc., and can solve the problems of single color and long response time.
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Embodiment 1
[0026]
[0027] Preparation of pink electrochromic material 1: Under the protection of nitrogen, 0.3 g (0.6 mmol) of compound a (synthesis method reference H. Zhang, B. Tieke, Polym. Chem. 2014, 5 , 6391–6406) and 0.33 g (2.4 mmol) of potassium carbonate dissolved in 10 mL N , N -Dimethylformamide, then add 0.46 g (2.4 mmol) of 1-bromo-6-methylheptane, heat to 80 °C, and react for 24 hours. After the reaction is complete, pour the reaction system into water and wash with acetic acid Ethyl ester extraction, the organic phase was washed three times with water, the solvent was removed after drying, and 259 mg of compound b was obtained by column separation and purification, with a yield of 60%. Then, under nitrogen protection, 252 mg (0.35 mmol) b, 289 mg (1.0 mmol) triphenylamine boronic acid were dissolved in 20 mL tetrahydrofuran, and 15 mL saturated potassium carbonate aqueous solution and 58 mg (0.05 mmol) Pd(PPh 3 ) 4 , heated to 85 ° C, after 8 hours of reaction, t...
Embodiment 2
[0031] Preparation of purple electrochromic material 2: under nitrogen protection, 133 mg (0.185 mmol) b (see Example 1 for the synthesis method), 240 mg (0.556 mmol) p-methoxytriphenylamine borate and 2.8 g ( 20 mmol) of potassium carbonate was dissolved in 30 mL of toluene and 10 mL of water, and 35 mg (0.03 mmol) of Pd(PPh 3 ) 4 , heated to 85 ° C, after 10 hours of reaction, the reaction system was poured into water, extracted with dichloromethane, the organic phase was washed three times with water, dried, spin-dried to remove the solvent, and purified by column separation to obtain 107 mg of compound 2 with a yield of 50 %.
[0032]
[0033] Select FTO conductive glass as the anode and cathode transparent conductive substrates, protect the surface of the FTO glass conductive layer that does not need to be etched with adhesive tape, spread zinc powder on the surface of the FTO glass conductive layer that needs to be etched, and then drop concentrated hydrochloric acid...
Embodiment 3
[0036] Preparation of green electrochromic material 3: under nitrogen protection, 73 mg (0.102 mmol) b (see Example 1 for the synthesis method) and 300 mg (0.408 mmol) p-methoxytriphenylamine ethylene dioxythiophene tin reagent were dissolved In 20 mL of N,N-dimethylformamide (DMF), add 20 mg (0.017 mmol) of Pd(PPh 3 ) 4 , heated to 100 ° C, after 6 hours of reaction, the reaction system was poured into water, extracted with dichloromethane, the organic phase was washed three times with water, dried, spin-dried to remove the solvent, and purified by column separation to obtain 88 mg of compound 3 with a yield of 60 %.
[0037]
[0038] Select ITO conductive glass as the anode and cathode transparent conductive substrates, protect the surface of the ITO glass conductive layer that does not need to be etched with adhesive tape, immerse in hydrochloric acid (5 M) at 50 ℃, and take out the etched ITO glass after 100 seconds , washed with deionized water and then blown dry wit...
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