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Self-assembly preparation of organic/inorganic compound film by transient metal substitution of polyoxometallate and polyamide-amine

A polyoxometalate, transition metal technology, applied in the field of organic-inorganic composite thin film preparation, achieves the effects of high stability, simple operation, and short film-forming time

Inactive Publication Date: 2011-03-30
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, some TMSP-organic self-assembled supramolecular thin films have been prepared by using the layer-by-layer self-assembly method, using TMSP as the inorganic anion and simple chain organic matter as the cation, but containing transition metal substituted polyoxometalates and spherical molecules- The functional film of polyamide-amine has not been reported yet

Method used

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  • Self-assembly preparation of organic/inorganic compound film by transient metal substitution of polyoxometallate and polyamide-amine

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 1. Cleaning:

[0021] Sonically clean the conductive glass substrate in acetone solution for 5 minutes, take it out and rinse it with distilled water, immerse it in NaOH solution and ultrasonically clean it for 5 minutes, take it out and rinse it with distilled water, and dry it with nitrogen gas to get the cleaned conductive glass substrate for use.

[0022] 2. Cationization:

[0023] The cleaned conductive glass substrate was immersed in 1% (wt%, mass fraction) PDDA solution for 30 minutes, rinsed with deionized water, and dried with nitrogen to obtain a cationized conductive glass substrate.

[0024] 3. Film self-assembly:

[0025] Put the cationized conductive glass substrate in 5mmol·L -1 PMo 11 In the solution of Cu, within the potential range of -0.1 ~ 0.65V, at 100mV s -1 The scanning speed was scanned for 25 weeks, and then washed with ethanol solution and deionized water and placed in 1% (wt%) PAMAM solution at 100mV·s -1 The speed scan scans for 25 weeks...

Embodiment 2

[0029] 1. Cleaning:

[0030] The glassy carbon electrode substrates were sequentially coated with 1.0, 0.3 and 0.05 μm α-Al 2 o 3 Powder polishing, ultrasonic cleaning in ethanol solution and distilled water for 10min, at 0.5mol L -1 h 2 SO 4 Control the potential range of -0.1 to 0.65V in the solution for cyclic potential scanning until a stable standard cyclic voltammogram is obtained.

[0031] 2. Cationization:

[0032] Place the cleaned glassy carbon electrode substrate in 5mmol·L -1 Soak in the ethanol solution of p-aminothiophenol for 15 hours, take it out, wash it with distilled water, and dry it with nitrogen to obtain a cationized glassy carbon electrode substrate.

[0033] 3. Film self-assembly:

[0034] Put the cationized glassy carbon electrode substrate in 5mmol·L -1 PMo 11 In the solution of Cu, in the range of potential -0.1 ~ 0.65V at 100mV s -1 The scanning speed was scanned for 25 weeks, washed with ethanol solution and deionized water, and then pla...

Embodiment 3

[0037]The specific preparation method is with reference to the preparation process of the multilayer composite thin film in embodiment 1, and the X-ray photoelectron spectrum of thin film and atomic force microscope characterization result show that this method has successfully prepared PMo 11 Compared with the traditional immersion method, the Cu / PAMAM multilayer composite film has a simple preparation process, a short time, and better uniformity of the prepared film.

[0038] The cyclic voltammetric behavior test result of different layers thin films shows that the PMo prepared by the method in embodiment 2 11 Compared with the traditional immersion method, the Cu / PAMAM composite film has better uniformity, higher order and better reproducibility.

[0039] With reference to the composite film prepared by the method of Example 1 and Example 2, in the potential range of -0.1-0.65V, 0.5mol L -1 H 2 SO 4 , at a scan rate of 0.1V·s -1 After 50 scans, only 2.7% of the peak cur...

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Abstract

This invention relates to a preparation method of an organic-inorganic composite film which is self-mounted from transitional metal substituted polyoxometallate and Polyamide (PI)-amine tree-form molecule and is provided with electrocatalysis activity. The technical proposal is: a glassy carbon electrode or conductive glass substrate is cleaned and then go through cationization to obtain a ready-for-use substrate filmed by the glassy carbon electrode or the conductive glass substrate; the ready-for-use substrate is alternatively immerged into the transitional metal substituted polyoxometallate solution and PAMAM tree-form molecule for circulating scanning, so as to complete the self mounting of the film. By repeating the above steps, the organic-inorganic composite film with different layer numbers can be prepared. The composite film prepared by the method of the invention has the advantages of simple operation, short filming time and good uniformity, and the composite film reserves various electrochemical properties of TMPS. In particular, by using the PAMAM tree form molecule as the organic cation, the composite film is provided with high stability and high permeability. The composite film is expected to be applied to chemically modified electrodes and environmental catalysis.

Description

technical field [0001] The invention relates to the preparation of an organic-inorganic composite thin film, in particular to the preparation of a transition metal substituted polyoxometalate and polyamide-amine dendrimer self-assembled organic-inorganic composite thin film with electrocatalytic activity. Background technique [0002] The development of modern science and technology, especially information technology, electronic technology, photonic technology and ultra-large-scale integration technology, drives the structure of devices to develop in the direction of miniaturization, integration, multi-function and high reliability, and the intelligentization of materials and thin films put forward higher and higher requirements. The organic-inorganic composite film combines organic matter and inorganic matter at the molecular level, so that the material has both the flexible characteristics of organic matter and the rigidity of inorganic matter. At present, organic-inorgan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C17/00
Inventor 林深罗明洪张晓凤
Owner FUJIAN NORMAL UNIV
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