Preparation method of porous film with regular vertical pores

A technology of vertical channels and porous membranes, which is applied in the field of preparation of porous membranes with regular vertical channels, which can solve the problems of wide distribution of pore size and disordered channels, and achieve the effect of simple method, easy operation and good hydrophilicity

Inactive Publication Date: 2013-11-27
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is simple, does not involve chemical reactions, has no mass loss, and can change the size of the pores by changing the swelling conditions, but the previous work is to directly swell the spin-coated film, and the resulting pores are disordered and the distribution of the pore size is relatively wide.

Method used

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  • Preparation method of porous film with regular vertical pores
  • Preparation method of porous film with regular vertical pores
  • Preparation method of porous film with regular vertical pores

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (a) Use a balance to weigh 0.06 g of a block copolymer of polystyrene and poly(2-vinylpyridine) (the volume ratio of poly(2-vinylpyridine) is 20%, and the total molecular weight is 362,000 Daltons) , be dissolved in 2.0 grams of chloroform, be mixed with the solution that polymer mass fraction is 4%;

[0030] (b) After the polymer is completely dissolved, filter the solution with a PTFE filter head to remove large aggregates, and then coat the polymer solution on the silicon substrate on a spin coater at 2000 rpm;

[0031] (c) Transfer the film to a small bottle with chloroform at the bottom of the bottle, anneal the film in the vapor of chloroform for 10 minutes, take it out, and dry it naturally in the air;

[0032] (d) The annealed film was immersed in ethanol at different temperatures (40, 45, 50, 55, 60, 70°C) to swell for 3 hours and then taken out, and the ethanol was allowed to evaporate and dry naturally in the air.

[0033] It can be seen from Figure (1) that...

Embodiment 2

[0036] (a) Weigh 0.06 g of block copolymer of polystyrene and polyacrylic acid (polyacrylic acid) with a volume ratio of 25% and a total molecular weight of 66,500 Daltons) with a balance, dissolve it in 3.0 g of tetrahydrofuran, and prepare a polymerized The substance mass fraction is 2% solution;

[0037] (b) After the polymer is completely dissolved, filter the solution with a PTFE filter head to remove large aggregates, and then coat the polymer solution on the silicon substrate on a spin coater at 3000 rpm;

[0038] (c) Transfer the film to a small bottle with toluene at the bottom of the bottle, anneal the film in toluene vapor for 40 seconds, take it out, and dry it naturally in the air;

[0039] (d) After the annealed film was immersed in ethylene glycol at 30°C and swelled for 12 hours, it was taken out, and the ethylene glycol was allowed to evaporate and dry naturally in the air.

[0040] It can be seen from Figure (4a) that after swelling, a pore structure with un...

Embodiment 3

[0042] (a) Weigh 0.06 g of polyacrylonitrile and polyoxyethylene block copolymer (polyoxyethylene) with a volume ratio of 10% and a total molecular weight of 90,000 Daltons) with a balance, dissolve it in 0.6 g of toluene, and prepare Become the solution that polymer mass fraction is 10%;

[0043] (b) After the polymer is completely dissolved, filter the solution with a PTFE filter head to remove large aggregates, and then coat the polymer solution on the silicon substrate on a spin coater at 3000 rpm;

[0044] (c) Transfer the film to a small bottle with tetrahydrofuran at the bottom of the bottle, anneal the film in the steam of tetrahydrofuran for 1 hour, take it out, and dry it naturally in the air;

[0045] (d) After the annealed film is immersed in water at 80°C and swelled for 72 hours, it is taken out, and the water is allowed to evaporate and dry naturally in the air.

[0046] From the SEM image, it can be seen that a regular hexagonal circular channel structure is f...

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Abstract

The invention relates to a preparation method of a porous film with regular vertical pores. The preparation method comprises the following steps of: firstly, annealing a block copolymer film by using a solvent, inducing the block copolymer to generate phase separation so as to form a vertically oriented micro-phase structure; and then performing selective swelling on dispersed phases of the block copolymer by using a swelling agent, and changing a dispersed structure into a pore structure so as to form a porous film with a highly-ordered vertical pore structure. The film prepared by the method has a vertically-oriented cylindrical pore structure, the sizes of the pores are highly uniform, the arrangement is highly regular, and the pore diameter is adjustable. The preparation method is extremely simple and convenient to operate, and is controllable without chemical reactions, so that the preparation method has a wide application prospect in the fields of separation films, nano etching and the like.

Description

technical field [0001] The invention relates to a method for preparing a porous membrane with regular vertical channels, in particular to annealing a block copolymer film by a solvent to form a vertical microphase structure, and then selectively swelling the dispersed phase by a selective solvent to form a vertical microphase structure. regular pore structure. Background technique [0002] Block copolymers can undergo microphase separation to form a regular and ordered array of microphase structures. For block copolymer films, due to the joint action of the substrate and the free surface, the microphase formed by the copolymer film is usually parallel to the surface. Vertical microphase structures can be obtained by solvent annealing, but the height of vertical microphases obtained by solvent annealing reported in the literature usually does not exceed 100nm. [0003] Transforming the dispersed phase of block copolymer films with vertical microphases into channels can form...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08J7/02C08L53/00
Inventor 汪勇殷俊邢卫红范益群汪朝晖
Owner NANJING UNIV OF TECH
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