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A kind of preparation method of phosphoric acid-doped layer-by-layer self-assembled polymer composite film

A layer-by-layer self-assembly and self-assembled membrane technology, applied in fuel cells, electrical components, electrochemical generators, etc., to achieve the effects of improving electrical conductivity, improving proton conductivity, and good thermal stability

Active Publication Date: 2019-01-08
NORTHEASTERN UNIV LIAONING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] So far, although the research group of Professor N.A. Kotov of the University of Michigan has used self-assembly technology to prepare gold nanoparticles (Au nanoparticles) and polyurethane (PU) into a (PU / Au) with a thickness of 2 microns but a self-assembled structure of 500 layers. 500 Ultra-thin film, and our research group reported that PU and sulfonated polyether ether ketone (SPEEK) were used to prepare SPEEK / PU composite film by solution casting method, but the SPEEK / PU film with layer-by-layer self-assembly structure was prepared by layer-by-layer self-assembly technology , has not yet been reported

Method used

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  • A kind of preparation method of phosphoric acid-doped layer-by-layer self-assembled polymer composite film
  • A kind of preparation method of phosphoric acid-doped layer-by-layer self-assembled polymer composite film
  • A kind of preparation method of phosphoric acid-doped layer-by-layer self-assembled polymer composite film

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Embodiment 1

[0027] The preparation method of the phosphoric acid-doped layer-by-layer self-assembled polymer composite membrane of this embodiment is carried out according to the following steps:

[0028] (1) Add 76mL of deionized water to 2.35g of SPEEK with a sulfonation degree of 94.3%, at 70 o C carries out magnetic stirring, and the preparation volume fraction is the SPEEK homogeneous aqueous solution of 3%;

[0029] (2) Use piranha solution (300mL98% H 2 SO 4 , 100mL 30% H 2 o 2 ) The treated negatively charged glass sheet is put into the PU solution with a mass fraction of 3%, and soaked for 6 minutes;

[0030] (3) Take out the glass piece, soak it in deionized water for 20s, take it out and blow it until there is no water on the surface, soak it again in the SPEEK homogeneous aqueous solution in step (1), soak it for 6min, then soak it in deionized water for 20s, take it out and blow it out. Until the surface is dry, complete the self-assembly of PU and SPEEK, which is record...

Embodiment 2

[0036] The preparation method of the phosphoric acid-doped layer-by-layer self-assembled polymer composite membrane of this embodiment is carried out according to the following steps:

[0037] (1) Add 80 mL of deionized water to 0.81 g of SPEEK with a sulfonation degree of 94.3%, at 50 o C carries out magnetic stirring, and the preparation volume fraction is the SPEEK homogeneous aqueous solution of 1%;

[0038] (2) Use piranha solution (300mL98% H 2 SO 4 , 100mL 30% H 2 o 2 ) The treated negatively charged glass sheet is put into the PU solution with a mass fraction of 1%, and soaked for 6 minutes;

[0039] (3) Take out the glass piece, soak it in deionized water for 20s, take it out and blow it until there is no water on the surface, soak it again in the SPEEK homogeneous aqueous solution in step (1), soak it for 6min, then soak it in deionized water for 20s, take it out and blow it out. Until the surface is dry, complete the self-assembly of PU and SPEEK, which is reco...

Embodiment 3

[0044] The preparation method of the phosphoric acid-doped layer-by-layer self-assembled polymer composite membrane of this embodiment is carried out according to the following steps:

[0045] (1) Add 60 mL of deionized water to 3.16 g of SPEEK with a sulfonation degree of 45.3%, at 80 o C carries out magnetic stirring, and the preparation volume fraction is the SPEEK homogeneous aqueous solution of 5%;

[0046] (2) Use piranha solution (300mL98% H 2 SO 4 , 100mL 30% H 2 o 2 ) The treated negatively charged glass sheet is put into the PU solution with a mass fraction of 3%, and soaked for 6 minutes;

[0047] (3) Take out the glass piece, soak it in deionized water for 20s, take it out and blow it until there is no water on the surface, soak it again in the SPEEK homogeneous aqueous solution in step (1), soak it for 6min, then soak it in deionized water for 20s, take it out and blow it out. Until the surface is dry, complete the self-assembly of PU and SPEEK, which is reco...

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Abstract

The invention belongs to the technical field of fuel cells, and particularly relates to a preparation method of a phosphoric acid-doped layer by layer self-assembly polymer composite film. The preparation method comprises the following steps of firstly preparing an SPEEK (Sulfonated Polyether Ether Ketone) homogeneous phase water solution; putting a glass sheet into a PU (Poly Urethane) solution for soaking; taking the glass sheet out; soaking into deionized water; taking out, and blowing to realize no water on the surface; re-soaking in the SPEEK homogeneous phasewater solution; then soaking in the deionized water; blowing to realize no water on the surface; completing layer by layer self-assembly of PU and SPEEK; repeating for 170 to 200 times to obtain a (SPEEK / PU) 170 to 200 self-assembly film; after soaking a glass sheet carrying the (SPEEK / PU) 170 to 200 self-assembly film into a hydrofluoric acid solution for 10min, taking the (SPEEK / PU) 170 to 200 self-assembly film out; soaking the (SPEEK / PU) 170 to 200 self-assembly film into a PA water solution, and obtaining the phosphoric acid-doped (SPEEK / PU) 170 to 200 self-assembly film. According to the preparation method of the phosphoric acid-doped layer by layer self-assembly polymer composite film provide by the invention, a layer by layer self-assembly technology is utilized, so that a high-temperature proton exchange film with a layer by layer self-assembly structure, high proton conductivity, a favorable mechanical property and stabilityis prepared based on a polycation polymer and a polyanion polymer.

Description

technical field [0001] The invention belongs to the technical field of fuel cells, and in particular relates to a method for preparing a phosphoric acid-doped layer-by-layer self-assembled polymer composite membrane. Background technique [0002] Layer-by-layer self-assembly technology (layer-by-layer, LBL) is a simple and multifunctional surface modification method developed rapidly in the 1990s. Alternate deposition in solution to prepare polyelectrolyte self-assembled multilayer films. However, the earliest concept of self-assembly can be traced back to the 1960s. In 1966, DuPont scientist Iler used colloidal particles with opposite charges to construct a multilayer structure through alternate adsorption. It did not receive widespread attention at the time. Since then, with the deepening of research, self-assembly technology has gradually attracted the attention of researchers. In the 1980s, J. Sagiv reported the related research on the formation of two-dimensional ord...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M8/1018H01M8/1025H01M8/1041H01M8/1044H01M8/1069
CPCH01M8/1018H01M8/1025H01M8/1041H01M8/1044H01M8/1069Y02E60/50
Inventor 车全通于津铭程世成
Owner NORTHEASTERN UNIV LIAONING
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