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A kind of method for preparing ultra-thin organosilicon film
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An organosilicon and organosilicon source technology, applied in the field of preparation of ultra-thin organosilicon membranes, can solve the problems of small flux, "large membrane thickness, low film formation rate, etc., and achieve the effect of high flux or permeability.
Active Publication Date: 2018-05-01
CHANGZHOU UNIV
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[0005] Aiming at the problems of "large film thickness, small flux, low film formation rate, and difficult control of the process" existing in the dipping and pulling coating method commonly used in the current silicon film preparation process, the present invention provides a relatively simple ultra-thin film The preparation method of the organic silicon film adopts the thermal coating method to wipe and coat low-concentration organic silicon sol, and directly performs rapid calcination after coating the film to prepare an ultra-thin and complete organic silicon separation film with a separation layer thickness of less than 100nm.
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Embodiment 1
[0029] (1) Preparation of organosilica sol
[0030] Under the catalysis of hydrochloric acid, the organosilicon polymer sol was prepared through the hydrolysis polymerization reaction of the organosilicon source precursor BTESEthy, and its concentration was diluted to 0.3wt%;
[0031] (2) The outer tube type α-Al 2 o 3 The support body (50% porosity, average pore diameter 2μm, outer diameter 10mm, length 100mm) was preheated to 200°C and taken out, immediately dipped the pre-prepared silicon-zirconium sol (0.5wt%) with absorbent cotton, and supported it in one direction Quickly rub on the body, put it into a 550°C furnace for calcination for 20 minutes immediately after coating, repeat this process 4 times, and obtain the transition layer of the film;
[0032] (3) Take out the support body coated with the transition layer and calcined in step (2), after cooling to 200°C, use absorbent cotton to dip the BTESEthy organosilicon sol obtained in step (1) on the transition layer q...
Embodiment 2
[0034] (1) Preparation of organosilica sol
[0035] Under the catalysis of hydrochloric acid, the organosilicon polymer sol was prepared by the hydrolysis polymerization reaction of the organosilicon source precursor BTESE, and its concentration was diluted to 0.4wt%;
[0036] (2) The outer tube type α-Al 2 o 3 The support body (50% porosity, average pore diameter 2μm, outer diameter 10mm, length 100mm) was preheated to 200°C and taken out, immediately dipped the pre-prepared silicon-zirconium sol (0.5wt%) with absorbent cotton, and supported it in one direction Quickly rub on the body, put it into a 550°C furnace for calcination for 15 minutes immediately after coating, repeat this process 5 times, and obtain the transition layer of the film;
[0037] (3) Take out the support body coated with the transition layer and calcined in step (2), and after cooling to 200°C, use absorbent cotton to dip the BTESE organosilicon sol obtained in step (1) on the transition layer quickly ...
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Abstract
The invention belongs to the field of film material preparation, and in particular, relates to a preparation method of an ultrathin organosilicon film. Aiming at the problems that a common impregnation dip-coating method in a current silicon membrane preparation process has larger film thickness, smaller flux, low film forming rate, difficult control of the process and the like, the invention provides a relatively simple preparation method of the ultrathin organosilicon film; low-concentration organosilicon sol is smeared by a hot coating method, direct rapid calcining is carried out after film coating, and the ultrathin and complete organosilicon separation film with the thickness of less than 100 nm is prepared.
Description
technical field [0001] The invention belongs to the field of film material preparation, in particular to a preparation method of an ultra-thin organic silicon film. Background technique [0002] A large number of commercial organic membranes generally have the disadvantages of poor chemical stability and thermal stability, while organosilicon membranes have excellent hydrothermal stability and chemical stability, and their application prospects are very broad. [0003] with SiO-based 2 Like traditional inorganic silicon films, organosilicon (or organic-inorganic hybrid silicon) films are generally prepared by the sol-gel method, and coating methods usually include dipping and spin-coating methods. The commonly used dipping and pulling method is to immerse one side of the support in the pre-prepared sol. After dipping for a period of time, the support is pulled out of the sol at a certain speed. Under the action of viscosity and gravity, the sol moves along the A uniform li...
Claims
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