CN107867874B - Silica nano porous membrane with gradient porosity and preparation method thereof - Google Patents
Silica nano porous membrane with gradient porosity and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silicon dioxide nano porous membrane with gradually changed porosity and a preparation method thereof. The nano porous membrane has a membrane thickness of 100-500nm and comprises more than 3 layers of porous membranes with different spherical apertures, wherein the aperture of the bottom layer is 1-3nm, the aperture of the surface layer is 5-8nm, the spacing between the edges of the pores is 10-2nm from bottom to top, and the porosity is 30-35% to 60-70% from bottom to top; the method comprises the steps of mixing ethyl tetrasilicate and ethanol to obtain a mixed solution, dropwise adding a nitric acid aqueous solution into the mixed solution, stirring to obtain a silicon dioxide sol, adding cetyl trimethyl ammonium bromide into the silicon dioxide sol, stirring, aging to obtain a mixed sol, sequentially placing a substrate into the mixed sol containing the gradually increased cetyl trimethyl ammonium bromide, carrying out lifting coating for more than 3 times, airing, and annealing to obtain the target product. The coating has both wear resistance and super-hydrophilicity, and can be widely and commercially applied to the fields of antifogging, self-cleaning, wide-spectrum permeability increasing and the like.
Description
Technical Field
The invention relates to a nano porous membrane and a preparation method thereof, in particular to a silicon dioxide nano porous membrane with gradually changed porosity and a preparation method thereof.
Background
The super-hydrophilic surface has strong attraction with water molecules, water drops can quickly spread on the super-hydrophilic surface, surface pollutants can be favorably carried away, the condensation of the liquid drops is prevented, and therefore the self-cleaning and anti-fog functions are achieved. Based on this mechanism, self-cleaning glass has been developed for use in automotive rearview mirrors, windshields, glass curtain walls, solar glass panels, and the like. In addition, the antifogging function of the super-hydrophilic surface also provides an idea for visualization in a high-humidity environment. At present, some beneficial attempts and efforts are made to obtain super-hydrophilic materials, such as an article entitled "influence of surfactant concentration on the structure of nano mesoporous silica thin film", volume 2969-2972 of supplement (35) of 2004 functional materials. The shape of the pores in the nano mesoporous silica film mentioned therein is spherical or rod-like; when the preparation method is used, firstly, sol is prepared by adopting an acid/acid two-step method, then the silicon dioxide-surfactant mesoporous material transparent film is obtained by methods of pulling, quickly evaporating a solvent and the like, and then the heat treatment is carried out at the temperature of 400 ℃ to obtain a product. Firstly, the whole porosity of the product is single and constant from top to bottom, so that the hydrophilicity is not ideal when the porosity of the product is small, and the wear resistance is not good when the porosity is large, namely, the wear resistance and the hydrophilicity are difficult to be considered simultaneously; secondly, the preparation method does not allow to obtain a product having both good wear resistance and good hydrophilicity.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the silicon dioxide nano porous membrane with gradually changed porosity, which can simultaneously meet the requirements of wear resistance and super hydrophilicity.
The invention also provides a preparation method of the silica nano porous membrane with gradually changed porosity.
In order to solve the technical problem of the present invention, the technical scheme adopted is that the silica nanoporous membrane with gradually changed porosity is composed of a silica porous membrane attached to a substrate, and particularly:
the thickness of the silica porous membrane is 100-500nm, and the silica porous membrane consists of more than 3 layers of porous membranes with different spherical pore diameters;
the pore diameter of the bottom layer of the porous membrane with more than 3 layers of different spherical pore diameters is 1-3nm, the pore diameter of the surface layer is 5-8nm, the distance between the pore edges is 10-2nm from bottom to top, and the porosity is 30-35% to 60-70% from bottom to top.
As a further improvement of the silica nanoporous membrane with graded porosity:
preferably, the porosity is closed porosity.
Preferably, the substrate is a conductor, or a semiconductor, or an insulator.
In order to solve another technical problem of the present invention, another technical solution is adopted in that the preparation method of the silica nanoporous membrane with gradually changed porosity comprises a sol-gel method, and particularly comprises the following steps:
step 1, according to the molar ratio of ethyl orthosilicate, ethanol, nitric acid and water being 1: 8-10: 0.05-0.09: 3-5, firstly mixing and stirring ethyl tetrasilicate and ethanol to obtain a mixed solution, and then mixing and stirring nitric acid and water to obtain a nitric acid aqueous solution;
step 2, dropwise adding a nitric acid aqueous solution into the mixed solution, stirring at 55-65 ℃ for at least 2h to obtain a silica sol, adding 1-5 wt% of hexadecyl trimethyl ammonium bromide into the silica sol, stirring for at least 1h, and aging for at least 4d to obtain the mixed sol;
and 3, sequentially placing the substrate in mixed sol containing gradually increased hexadecyl trimethyl ammonium bromide for more than 3 times of lifting coating, airing to obtain a substrate with more than 3 layers of porous membranes with different spherical apertures attached on the surface, and then placing the substrate with more than 3 layers of porous membranes with different spherical apertures attached on the surface at 480-520 ℃ for annealing for at least 3 hours to obtain the silicon dioxide nano porous membrane with the gradually changed porosity.
As a further improvement of the preparation method of the silica nanoporous membrane with gradual porosity:
preferably, the stirring speed at the time of obtaining the silica sol is 750 r/min.
Preferably, the substrate is a conductor, or a semiconductor, or an insulator.
Preferably, the descending speed of the substrate is 100mm/min, the dipping time is 2min, and the pulling speed is 25-50mm/min when the coating film is pulled.
Preferably, after each pulling coating, the coating is dried at 120 ℃ for 10 min.
Compared with the prior art, the beneficial effects are that:
firstly, the cross section of the film in the prepared target product is respectively characterized by using a transmission electron microscope and an X-ray diffractometer, and the result shows that the target product is a porous film which is attached to a substrate and has a plurality of layers of different spherical apertures; wherein, the aperture of the bottom layer of the porous film is 1-3nm, the aperture of the surface layer is 5-8nm, the spacing between the pore edges is 10-2nm from bottom to top, and the porosity is 30-35% to 60-70% from bottom to top; the porous membrane is composed of silica. The target product assembled by the multilayer silicon dioxide with different spherical apertures has different spherical apertures and different pore distances, namely different porosities, so that the target product can not only utilize the small porosity structure of the bottom layer to enhance the adhesive force with the substrate, but also can exert the hydrophilicity of the large porosity structure of the surface layer, and further has both wear resistance and super-hydrophilicity.
Secondly, the preparation method is simple, scientific and efficient. The silicon dioxide nano porous membrane with the gradually changed porosity, which can simultaneously meet the requirements of wear resistance and super-hydrophilicity, is prepared, and has the characteristic of low preparation cost, so that the target product is extremely easy to be widely and commercially applied to the fields of fog prevention, self cleaning, wide-spectrum permeability increase and the like.
Drawings
Fig. 1 is one of results of characterization of cross-sections of thin films obtained by making different amounts of cetyltrimethylammonium bromide added according to the preparation method using Transmission Electron Microscopy (TEM). Wherein, a in FIG. 1 is a TEM image of the film when the amount of cetyltrimethylammonium bromide added is 1.5 wt%, from which it can be seen that the spherical pore diameter of the film is 1-2nm and the pore edge spacing is 6-7 nm; and b is a TEM image of the film at an addition amount of 4.5 wt% of cetyltrimethylammonium bromide, from which it can be seen that the spherical pore diameter of the film is 2-3nm and the pore edge spacing is 3-4 nm.
Detailed Description
Preferred embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
First commercially available:
ethyl tetrasilicate;
ethanol;
nitric acid;
deionized water as water;
conductors, semiconductors and insulators as substrates.
Then:
example 1
The preparation method comprises the following specific steps:
step 1, according to the molar ratio of ethyl orthosilicate, ethanol, nitric acid and water being 1: 8: 0.09: 3, firstly, mixing ethyl tetrasilicate and ethanol and stirring to obtain a mixed solution. Nitric acid and water are mixed and stirred to obtain nitric acid aqueous solution.
Step 2, dropwise adding a nitric acid aqueous solution into the mixed solution, and stirring for 4 hours at 55 ℃; wherein the stirring speed is 750r/min, and the silicon dioxide sol is obtained. And adding 1 wt%, 3 wt% and 5 wt% of hexadecyl trimethyl ammonium bromide into 3 parts of the silica sol, stirring for 1 hour, and aging for 4 days to obtain 3 parts of mixed sol.
Step 3, sequentially placing the substrate in mixed sol containing gradually increased hexadecyl trimethyl ammonium bromide for 3 times of lifting coating, and then airing; the substrate is one of insulators, namely a glass slide, the descending speed of the substrate is 100mm/min, the dipping time is 2min, the pulling speed is 25mm/min when the coating is pulled, and after the coating is pulled each time, the substrate is dried at 120 ℃ for 10min to obtain the substrate with 3 layers of porous membranes with different spherical apertures attached to the surface. And then the substrate with 3 layers of porous membranes with different spherical apertures attached on the surface is placed at 480 ℃ for annealing for 5 hours to prepare the silicon dioxide nano porous membrane with gradually changed porosity.
Example 2
The preparation method comprises the following specific steps:
step 1, according to the molar ratio of ethyl orthosilicate, ethanol, nitric acid and water being 1: 8.5: 0.08: 3.5, mixing ethyl tetrasilicate and ethanol and stirring to obtain a mixed solution. Nitric acid and water are mixed and stirred to obtain nitric acid aqueous solution.
Step 2, dropwise adding the nitric acid aqueous solution into the mixed solution, and stirring for 3.5 hours at 58 ℃; wherein the stirring speed is 750r/min, and the silicon dioxide sol is obtained. And adding 1 wt%, 2 wt%, 3 wt% and 5 wt% of hexadecyl trimethyl ammonium bromide into 4 parts of the silica sol, stirring for 1.3h, and aging for 4.5d to obtain 4 parts of mixed sol.
Step 3, sequentially placing the substrate in mixed sol containing gradually increased hexadecyl trimethyl ammonium bromide to carry out pulling coating for 4 times, and then airing; the substrate is one of insulators, namely a glass slide, the descending speed of the substrate is 100mm/min, the dipping time is 2min, the pulling speed is 31mm/min when the coating is pulled, and after the coating is pulled each time, the substrate is dried at 120 ℃ for 10min to obtain the substrate with 4 layers of porous membranes with different spherical apertures attached to the surface. And then the substrate with 4 layers of porous membranes with different spherical apertures attached to the surface is placed at 490 ℃ for annealing for 4.5h to prepare the silicon dioxide nano porous membrane with the gradually changed porosity.
Example 3
The preparation method comprises the following specific steps:
step 1, according to the molar ratio of ethyl orthosilicate, ethanol, nitric acid and water being 1: 9: 0.07: and 4, firstly, mixing ethyl tetrasilicate and ethanol, and stirring to obtain a mixed solution. Nitric acid and water are mixed and stirred to obtain nitric acid aqueous solution.
Step 2, dropwise adding a nitric acid aqueous solution into the mixed solution, and stirring for 3 hours at 60 ℃; wherein the stirring speed is 750r/min, and the silicon dioxide sol is obtained. And adding 1 wt%, 2 wt%, 3 wt%, 4 wt% and 5 wt% of hexadecyl trimethyl ammonium bromide into 5 parts of the silica sol, stirring for 1.5h, and aging for 5d to obtain 5 parts of mixed sol.
Step 3, sequentially placing the substrate in mixed sol containing gradually increased hexadecyl trimethyl ammonium bromide for 5 times of lifting coating, and then airing; the substrate is one of insulators, namely a glass slide, the descending speed of the substrate is 100mm/min, the dipping time is 2min, the pulling speed is 38mm/min when the coating is pulled, and after the coating is pulled each time, the substrate is dried at 120 ℃ for 10min to obtain the substrate with 5 layers of porous membranes with different spherical apertures attached to the surface. And then the substrate with 5 layers of porous membranes with different spherical apertures attached on the surface is placed at 500 ℃ for annealing for 4h to prepare the silicon dioxide nano porous membrane with gradually changed porosity.
Example 4
The preparation method comprises the following specific steps:
step 1, according to the molar ratio of ethyl orthosilicate, ethanol, nitric acid and water being 1: 9.5: 0.06: and 4.5, firstly, mixing ethyl tetrasilicate and ethanol, and stirring to obtain a mixed solution. Nitric acid and water are mixed and stirred to obtain nitric acid aqueous solution.
Step 2, dropwise adding the nitric acid aqueous solution into the mixed solution, and stirring at 63 ℃ for 2.5 hours; wherein the stirring speed is 750r/min, and the silicon dioxide sol is obtained. And then hexadecyl trimethyl ammonium bromide with the mass fractions of 1 wt%, 2 wt%, 3 wt%, 4 wt%, 4.5 wt% and 5 wt% is added into 6 parts of the silica sol respectively, and after stirring for 1.8h, the mixture is aged for 5.5d to obtain 6 parts of mixed sol.
Step 3, sequentially placing the substrate in mixed sol containing gradually increased hexadecyl trimethyl ammonium bromide for 6 times of lifting coating, and then airing; the substrate is one of insulators, namely a glass slide, the descending speed of the substrate is 100mm/min, the dipping time is 2min, the pulling speed is 44mm/min when the coating is pulled, and after the coating is pulled each time, the substrate is dried at 120 ℃ for 10min to obtain the substrate with 6 layers of porous membranes with different spherical apertures attached to the surface. And then the substrate with 6 layers of porous membranes with different spherical apertures attached to the surface is placed at 510 ℃ for annealing for 3.5h to prepare the silicon dioxide nano porous membrane with the gradually changed porosity.
Example 5
The preparation method comprises the following specific steps:
step 1, according to the molar ratio of ethyl orthosilicate, ethanol, nitric acid and water being 1: 10: 0.05: and 5, firstly, mixing ethyl tetrasilicate and ethanol, and stirring to obtain a mixed solution. Nitric acid and water are mixed and stirred to obtain nitric acid aqueous solution.
Step 2, dropwise adding a nitric acid aqueous solution into the mixed solution, and stirring at 65 ℃ for 2 hours; wherein the stirring speed is 750r/min, and the silicon dioxide sol is obtained. And adding 1 wt%, 1.5 wt%, 2 wt%, 3 wt%, 4 wt%, 4.5 wt% and 5 wt% of cetyltrimethylammonium bromide to 7 parts of the silica sol, stirring for 2 hours, and aging for 6 days to obtain 7 parts of mixed sol.
Step 3, sequentially placing the substrate in mixed sol containing gradually increased hexadecyl trimethyl ammonium bromide for carrying out lifting coating for 7 times, and then airing; the substrate is one of insulators, namely a glass slide, the descending speed of the substrate is 100mm/min, the dipping time is 2min, the pulling speed is 50mm/min when the coating is pulled, and after the coating is pulled each time, the substrate is dried at 120 ℃ for 10min to obtain the substrate with 7 layers of porous membranes with different spherical apertures attached to the surface. And then the substrate with 7 layers of porous membranes with different spherical apertures attached to the surface is placed at 520 ℃ for annealing for 3h to prepare the silicon dioxide nano porous membrane with gradually changed porosity.
Further, the above examples 1 to 5 were repeated using a conductor or a semiconductor or an insulator as a substrate, respectively, to produce a silica nanoporous film having a gradually changing porosity.
It is apparent that those skilled in the art can make various modifications and variations to the silica nanoporous membrane having a graded porosity of the present invention and the method of preparing the same without departing from the spirit and scope of the present invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (6)
1. A silica nanoporous membrane having a graded porosity comprised of a silica porous membrane attached to a substrate, characterized in that:
the thickness of the silica porous membrane is 100-500nm, and the silica porous membrane consists of more than 3 layers of porous membranes with different spherical pore diameters;
the pore diameter of the bottom layer of the porous membrane with more than 3 layers of different spherical pore diameters is 1-3nm, the pore diameter of the surface layer is 5-8nm, the distance between the pore edges is 10-2nm from bottom to top, and the porosity is 30-35% to 60-70% from bottom to top;
the preparation method of the nano porous membrane comprises the following steps:
step 1, according to the molar ratio of ethyl orthosilicate, ethanol, nitric acid and water being 1: 8-10: 0.05-0.09: 3-5, firstly mixing and stirring ethyl tetrasilicate and ethanol to obtain a mixed solution, and then mixing and stirring nitric acid and water to obtain a nitric acid aqueous solution;
step 2, dropwise adding a nitric acid aqueous solution into the mixed solution, stirring at 55-65 ℃ for at least 2h to obtain a silica sol, adding 1-5 wt% of hexadecyl trimethyl ammonium bromide into the silica sol, stirring for at least 1h, and aging for at least 4d to obtain the mixed sol;
and 3, sequentially placing the substrate in mixed sol containing gradually increased hexadecyl trimethyl ammonium bromide for more than 3 times of lifting coating, airing to obtain a substrate with more than 3 layers of porous membranes with different spherical apertures attached on the surface, and then placing the substrate with more than 3 layers of porous membranes with different spherical apertures attached on the surface at 480-520 ℃ for annealing for at least 3 hours to obtain the silicon dioxide nano porous membrane with the gradually changed porosity.
2. The silica nanoporous membrane having a graded porosity as claimed in claim 1, characterized in that the porosity is a closed porosity.
3. The silica nanoporous membrane having a graded porosity as claimed in claim 1, wherein the substrate is a conductor, or a semiconductor, or an insulator.
4. The silica nanoporous membrane having a graded porosity as claimed in claim 1, wherein the stirring speed when obtaining the silica sol is 750 r/min.
5. The silica nanoporous membrane having a graded porosity according to claim 1, wherein the substrate is lowered at a speed of 100mm/min, the dipping time is 2min, and the pulling speed is 25 to 50mm/min when the coating film is pulled.
6. The silica nanoporous membrane having a graded porosity as claimed in claim 1, wherein the coating film is dried at 120 ℃ for 10min after each pulling-up.
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| CN109081608B (en) * | 2018-08-22 | 2021-04-09 | 上海西源新能源技术有限公司 | SiO for outdoor use2Super-hydrophilic nano coating and preparation method thereof |
| CN109081607A (en) * | 2018-08-22 | 2018-12-25 | 上海西源新能源技术有限公司 | Durable hydrophilic property SiO2The preparation method of mesoporous nano coating |
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| CN102964067A (en) * | 2012-12-11 | 2013-03-13 | 天津耀皮工程玻璃有限公司 | SiO2 antireflection film for solar photovoltaic glass and preparation method thereof |
| CN103964450A (en) * | 2013-02-01 | 2014-08-06 | 中国科学院理化技术研究所 | Preparation method of nano silicon dioxide particles with small particle size |
| CN104386919A (en) * | 2014-10-18 | 2015-03-04 | 中山市创科科研技术服务有限公司 | Glass with silicon dioxide sol antireflecting film and preparation method |
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| CN103964450A (en) * | 2013-02-01 | 2014-08-06 | 中国科学院理化技术研究所 | Preparation method of nano silicon dioxide particles with small particle size |
| CN104386919A (en) * | 2014-10-18 | 2015-03-04 | 中山市创科科研技术服务有限公司 | Glass with silicon dioxide sol antireflecting film and preparation method |
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