Unlock instant, AI-driven research and patent intelligence for your innovation.

High-efficiency electrochemical polymerization preparation and application of ruthenium complex film

A ruthenium complex, electrochemical technology, applied in the field of electrochemistry, to achieve the effect of broad application prospects

Inactive Publication Date: 2018-10-19
BEIJING NORMAL UNIVERSITY
View PDF3 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used electrochemical polymerization groups include thiophene [Wang Kezhi, Yang Wei, Xue Longxin, Preparation method and photoelectrochemical properties of electropolymerized thin films containing thienyl mononuclear ruthenium complexes, patent number: ZL201510641584.5.], triphenylamine [B.B. Cui, Z.Mao, Y.Chen, Y.W.Zhong, G.Yu, C.Zhan, J.Yao, Tuning of resistive memory switching in electropolymerized metallopolymeric films, Chem.Sci., 2015, 6, 1308.], carbazole[ Y. Zhu, C. Gu, S. Tang, T. Fei, X. Gu, H. Wang, Z. Wang, F. Wang, D. Lu, Y. Ma, J. Mater. Chem., 2009, 19 ,3941.] and pyrrole [M.Dakkach, X.Fontrodona, T.Parella, A.Atlamsani, I.Romero, M.Rodríguez, Dalton Trans., 2014,43,9916.], etc., and the complex is the use of two The two-point polymerization of a polymerizable group, and the three-point polymerization of ruthenium complexes have rarely been reported[]

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • High-efficiency electrochemical polymerization preparation and application of ruthenium complex film
  • High-efficiency electrochemical polymerization preparation and application of ruthenium complex film
  • High-efficiency electrochemical polymerization preparation and application of ruthenium complex film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, the preparation of ligand L

[0020] The synthetic route of ligand L is as follows:

[0021]

[0022] 210mg (1.0mmol) of 1,10-phenanthroline-5,6-dione, 389mg (1.5mmol) of 4-diphenylaminobenzaldehyde, 385mg (5.0mmol) of ammonium acetate and 93mg (1mmol) of aniline Suspended in 10mL of acetic acid. The mixture was refluxed at 110°C for 12h under the protection of nitrogen, then poured into 100mL of water, and adjusted to pH = 7 with ammonia water. The yellow precipitate obtained by filtration was recrystallized with a suitable solvent, and purified by silica gel column chromatography to obtain 540mg of the target product (50% yield). 1 H NMR (δ,ppm,400MHz,DMSO-d 6 ):9.08(d,J=4.0Hz,1H),9.01(d,J=8.0Hz,1H),8.94(d,J=4.0Hz,1H),7.87(q,J=4.0Hz,1H), 7.71-7.79(m,5H),7.47(d,J=12Hz,3H),7.29-7.37(m,5H),7.12(t,J=4.0Hz,2H),7.06(d,J=8.0Hz, 4H), 6.83(d, J=8Hz, 2H). ESI-MS mass spectrometry (Triple TOF TM 5600 + MSin CH 3 OH): Calculated value, m / z=540(M+H + ); ex...

Embodiment 2

[0023] Embodiment two, ruthenium complex [RuL 3 ](ClO 4 ) 2 preparation of

[0024] Ruthenium complex [RuL 3 ](ClO 4 ) 2 The synthetic route of is as follows:

[0025]

[0026] 26 mg (0.1 mmol) RuCl 3 ·3H 2 O and 161.7mg (0.3mmol) of L were suspended in 20mL ethanol. After the mixture was refluxed under nitrogen protection for 12 hours, the saturated aqueous solution of sodium perchlorate was added dropwise to precipitate the product, and finally 130mg of the target complex was obtained by silica gel column chromatography. The yield 68%. Proton NMR spectrum (δ, ppm, 600MHz, DMSO-d 6 ):9.08-9.14(m,3H),8.02(td,J 1 =12Hz,J 2 =6Hz,3H),7.86-7.94(m,3H),7.68-7.94(m,19H),7.42-7.47(m,8H),7.30-7.34(m,14H),7.09-7.12(m,7H) , 7.02-7.04 (m, 12H), 6.80 (q, J=6Hz, 6H). Mass Spectrum: (Triple TOF TM 5600 + MS, methanol): calculated value, m / z: 859 ([M-2ClO 4 - ] 2+ ); experimental value, m / z: 858 (100%).

Embodiment 3

[0027] Embodiment 3, the preparation of ruthenium complex electropolymerization film and the ultraviolet-visible absorption spectrum measurement of film

[0028]1. Clean indium-tin oxide (ITO) conductive glass. The ITO glass was cut into small pieces of 1.5 cm x 5 cm. Sequentially use detergent, one time of water ultrasonic cleaning three times each, each time for 5 minutes, and finally use the mixed solution of concentrated ammonia water: hydrogen peroxide: primary water (v:v:v, 1:1:5) at 70°C for half an hour . After taking it out, use water to ultrasonically clean it again, and finally use the ear washing ball to dry it and put it into a small bottle, and dry it for later use.

[0029] 2. Dissolve the ruthenium complex in 0.1M tetrabutylammonium hexafluorophosphate dichloromethane solution, the concentration of the ruthenium complex is 1mM, use ITO as the working electrode, the platinum electrode as the counter electrode, and the silver wire as the reference electrode, N...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method and electrochemical and photoelectrochemical properties of an electropolymerized film containing a triphenylamine-based mononuclear ruthenium complex, anda simple electrochemical method is used to form a polymer film from the mononuclear ruthenium complex on an ITO electrode. A test on the electrochemical properties of the film shows that a 1-5-ring film polymerized by the polymer has a thickness visible to naked eyes, and a test on the photoelectric properties of the film shows that in a negative bias portion, the negative an applied bias voltageis, the bigger the photocurrent of the film is, when the applied bias voltage is a positive value, the amplitude of variation of the photocurrent of the film is significantly smaller than the photocurrent when the applied bias voltage is a negative bias, and good rectification properties can be shown. Therefore, the triphenylamine-group-containing mononuclear ruthenium complex electropolymerized film has broad application prospects in the field of energy conversion.

Description

technical field [0001] The invention belongs to the field of electrochemistry, and relates to a preparation method of an electropolymerization film of a triphenylamine-containing mononuclear ruthenium complex and its electrochemical and photoelectrochemical properties. Background technique [0002] Electrochemical polymerization is a method of preparing functional polymer films by using the oxidation or reduction coupling reaction of precursor molecules at the interface of electrodes or solutions. This method can be used to adjust the doping degree and morphology of the film to obtain functional polymer film materials with rich properties and structures; at the same time, electrochemical polymerization occurs at the electrode / solution interface, which can The research system of interface chemistry can be enriched and new physical models can be provided by in-depth research on the mechanism and process. Electrochemical polymerization technology has developed rapidly in recen...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C08G61/12H01L51/00
CPCC08G61/123C08G2261/92C08G2261/3241C08G2261/374H10K85/111
Inventor 王克志王浩张语嫣张承成成婧荣
Owner BEIJING NORMAL UNIVERSITY