Preparation method for electro polymerization membrane comprising thienyl mononuclear ruthenium complex and photo electrochemical properties

A ruthenium complex, thienyl ruthenium technology, applied in the field of electrochemistry, can solve the problems of hindered, electrochemically unstable charge transport of polymeric materials, etc., and achieve the effect of wide application prospects

Inactive Publication Date: 2016-03-09
BEIJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the irreversible reduction process of some pure organic polymers, the electrochemical instability and charge transport of polymer materials are hindered [C.Groves, J.C.Blakesley, N.C.Greenham, Effect of charge trapping on geminate recombination and polymer solar cell performance, NanoLett., 2010, 10, 1063- 1069.]

Method used

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  • Preparation method for electro polymerization membrane comprising thienyl mononuclear ruthenium complex and photo electrochemical properties
  • Preparation method for electro polymerization membrane comprising thienyl mononuclear ruthenium complex and photo electrochemical properties
  • Preparation method for electro polymerization membrane comprising thienyl mononuclear ruthenium complex and photo electrochemical properties

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1, the preparation of ligand L

[0021] The synthetic route of ligand L is as follows:

[0022]

[0023] Compound 1 was prepared according to the literature [Z.H.Peng, A.R.Gharavi, L.P.Yu, Synthesis and characterization of photorefractive polymers containing transition metal complexes photosensitizer, J. Am. Chem. Soc., 1997, 119(20), 4622-4632.].

[0024] Compound 1 (0.33g, 0.72mmol) and thiophenecarbaldehyde (0.188g, 1.68mmol) were dissolved in 10ml of tetrahydrofuran, and under a nitrogen atmosphere, 10ml of t-BuOK (0.18g) suspension was slowly added dropwise to In the above solution, the solution changed from light yellow to dark red at this time, and the upper liquid surface glowed blue. After the dropwise addition, continue to stir at room temperature for 12h, and the system turns bright yellow. After the reaction was completed, the reaction system was poured into 300ml of dichloromethane, washed with water three times, dried over sodium sulfate an...

Embodiment 2

[0026] Embodiment two, ruthenium complex [Ru(bpy) 2 L](ClO 4 ) 2 preparation of

[0027] Ruthenium complex [Ru(bpy) 2 L](ClO 4 ) 2 The synthetic route of is as follows:

[0028]

[0029] Ru(bpy) 2 Cl 2 According to the literature [Z.Q.Ji, S.D.Huang, A.R.Guadalupe., Synthesis, X-ray structures, spectroscopic and electrochemical properties of ruthenium (II) complexes containing 2, 2'-bipyrimidine. Inorg. Chim. Acta, 2000, 305, 127-134.] method preparation.

[0030] Dissolve 50mg (0.19mmol) of Ligand L in 6ml of DMF, then add 10ml of ethanol and 88mg (0.23mmol) of Ru(bpy) 2 Cl 2 , N 2 Heating to reflux under protection for 20 hours, cooling to room temperature, suction filtration to remove unreacted ligands, spin out the ethanol in the filtrate, add sodium perchlorate aqueous solution to it, suction filtration to collect the precipitate, and vacuum dry the precipitate Then add a small amount of acetonitrile to dissolve it, then peroxide column, the developer is dichlo...

Embodiment 3

[0034] Embodiment three, the preparation of ruthenium complex electropolymerization thin film

[0035] 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 concentrated ammonia water: hydrogen peroxide: primary water = 1:1:5 (v:v:v) in a mixed solution of 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.

[0036] 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 into the solution 2 , pass 15min, after the end, with the...

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Abstract

The present invention discloses a preparation method for an electro polymerization membrane comprising a thienyl mononuclear ruthenium complex, electrochemistry thereof, and photo electrochemical properties. A simple electrochemical method is adopted, so that a mononuclear ruthenium complex form a polymer membrane on an ITO electrode, and a test on electrochemical properties of the membrane shows that a 20-ring membrane aggregated by the polymer has good stability in an aqueous solution. A test on photoelectric properties of the membrane shows that in a negative bias voltage partial, the negative the bias voltage is, the larger the photocurrent of the membrane is, and when the bias voltage is 0 V, an extremely large photocurrent is also shown; and along with the increase of the bias voltage, the change range of the photocurrent is significantly smaller than the photocurrent in a bias voltage, and an excellent rectifying property is showed. Therefore, the electro polymerization membrane comprising the thienyl mononuclear ruthenium complex in the present invention has a broad application prospect 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 electropolymerized thin film containing a thienyl mononuclear ruthenium complex and its electrochemical and photoelectrochemical properties. Background technique [0002] In recent years, polymer films have aroused the interest of researchers because of their simple preparation method and superior performance compared with monomers. In optoelectronic devices, materials with efficient light absorption, charge separation and charge transfer transport functions are extremely important [A. Facchetti, π-Conjugated polymers for organic electronics and photovoltaic cell applications, Chem. Mater., 2011, 23, 733-758]. However, due to the irreversible reduction process of some pure organic polymers, the electrochemical instability and charge transport of polymer materials are hindered [C.Groves, J.C.Blakesley, N.C.Greenham, Effect of charge trapping on geminate rec...

Claims

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Application Information

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IPC IPC(8): C08G61/12H01L51/00
CPCC08G61/126C08G2261/3229C08G2261/92H10K85/113
Inventor 王克志杨薇薛龙新
Owner BEIJING NORMAL UNIVERSITY
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