CN107867874A - Silica nanometer perforated membrane with graded porosity and preparation method thereof - Google Patents
Silica nanometer perforated membrane with graded porosity and preparation method thereof Download PDFInfo
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- CN107867874A CN107867874A CN201711068784.1A CN201711068784A CN107867874A CN 107867874 A CN107867874 A CN 107867874A CN 201711068784 A CN201711068784 A CN 201711068784A CN 107867874 A CN107867874 A CN 107867874A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62222—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic coatings
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
Abstract
The invention discloses a kind of silica nanometer perforated membrane with graded porosity and preparation method thereof.The thickness of nano-porous films is 100 500nm, it is made up of the perforated membrane in more than 3 layers of different spherical apertures, wherein, bottom aperture is 1 3nm, top layer aperture is 5 8nm, bore edges spacing is 10 2nm from bottom to top, and porosity is 30 35% to 60 70% from bottom to top；Method is that tetrasilicic acid ethyl ester and ethanol first are mixed to get into mixed solution, aqueous solution of nitric acid is instilled dropwise again in mixed solution after stirring obtains silicon dioxide gel, cetyl trimethylammonium bromide is added thereto and is stirred, mixed sols is obtained through aging, afterwards, first substrate is sequentially placed into after including the lifting plated film that cetyl trimethylammonium bromide gradually carries out more than 3 times in increased mixed sols, dried, it is annealed again, purpose product is made.It is provided simultaneously with wearability and Superhydrophilic, can be extremely easy to widely commercial applications in the field such as antifog, automatically cleaning, wide range be anti-reflection.
Description
Technical field
The present invention relates to a kind of nano-porous films and preparation method, especially a kind of silica with graded porosity
Nano-porous films and preparation method thereof.
Background technology
There is strong attraction, water droplet can quickly be sprawled thereon, is advantageous between ultra-hydrophilic surface and hydrone
Take away surface contaminant and prevent Drop Condensation, so as to have automatically cleaning and antifog function.Based on this mechanism, people are
Self-cleaning glass is have developed, for occasions such as automobile rearview mirror, windshield, glass curtain wall, solar energy glass panels.This
Outside, the anti-fog function of ultra-hydrophilic surface also provides thinking for the visualization under high humidity environment.At present, people are in order to obtain super parent
Water material, some good tries and effort are made, " surfactant concentration is to mesoporous nano silicon dioxide film knot Ru entitled
The influence of structure ",《Functional material》The article of the 2969-2972 pages of supplementary issue (35) volume in 2004.The mesoporous nano referred in this article
Hole shape in silica membrane is spherical or bar-shaped；Colloidal sol is first prepared using acid/sour two-step method during preparation, then it is fast by lifting
After the methods of fast evaporation solvent obtains silica-surfactant mesoporous material transparent membrane, it is carried out at 400 DEG C of heat
Reason, obtain product.Though this product has the performance of surface hydrophilic, with its preparation method all there is weak point, first,
The overall porosity of product is single constant from top to bottom, and this is resulted in when product porosity, and hydrophily is undesirable,
And porosity it is larger when wearability it is bad, that is, be difficult to take into account wearability and hydrophily simultaneously；Secondly, preparation method can not obtain both
Have good wearability, hydrophily and good product.
The content of the invention
The technical problem to be solved in the present invention is to overcome weak point of the prior art, there is provided one kind can meet resistance to simultaneously
The silica nanometer perforated membrane with graded porosity of mill property and Superhydrophilic.
The invention solves another technical problem received to provide a kind of above-mentioned silica with graded porosity
The preparation method of rice perforated membrane.
To solve the technical problem of the present invention, used technical scheme is that the silica with graded porosity is received
Rice perforated membrane is made up of the porous silica film invested in substrate, particularly：
The thickness of the porous silica film is 100-500nm, its by more than 3 layers of different spherical apertures perforated membrane
Composition；
The bottom aperture of more than the 3 layers different spherical aperture perforated membranes is 1-3nm, top layer aperture is 5-8nm, bore edges
Spacing is 10-2nm from bottom to top, and porosity is 30-35% to 60-70% from bottom to top.
Further improvement as the silica nanometer perforated membrane with graded porosity：
Preferably, porosity is to close porosity.
Preferably, substrate is conductor, or semiconductor, or insulator.
To solve another technical problem of the present invention, another used technical scheme is, above-mentioned to have gradual change hole
The preparation method of the silica nanometer perforated membrane of gap rate includes sol-gal process, and it is as follows particularly to complete step：
Step 1, it is 1 according to the mol ratio of tetrasilicic acid ethyl ester, ethanol, nitric acid and water：8-10：0.05-0.09：3-5 ratio
Tetrasilicic acid ethyl ester and ethanol, are first mixed and stirred for, obtain mixed solution by example, then nitric acid and water are mixed and stirred for, and obtain nitre
Aqueous acid；
Step 2, first aqueous solution of nitric acid is instilled in mixed solution dropwise, and at least 2h is stirred at 55-65 DEG C, obtain two
Silica sol, then add mass fraction into silicon dioxide gel and be 1-5wt% cetyl trimethylammonium bromide, and stir
After mixing at least 1h, aging at least 4d, mixed sols is obtained；
Step 3, first substrate is sequentially placed into and includes cetyl trimethylammonium bromide and gradually enter in increased mixed sols
After the lifting plated film that row is more than 3 times, dry, obtain the substrate of the different spherical aperture perforated membrane of the attached above that haves three layers in surface, then by table
The substrate of the different spherical aperture perforated membranes of the attached above that haves three layers in face is placed at 480-520 DEG C at least 3h that anneals, and being made has gradual change hole
The silica nanometer perforated membrane of gap rate.
Further improvement as the preparation method of the silica nanometer perforated membrane with graded porosity：
Preferably, mixing speed when obtaining silicon dioxide gel is 750r/min.
Preferably, substrate is conductor, or semiconductor, or insulator.
Preferably, lift plated film when substrate decrease speed be 100mm/min, dip time 2min, pull rate be
25-50mm/min。
Preferably, 120 DEG C, 10min drying and processing are carried out to it after lifting plated film every time.
It is relative to the beneficial effect of prior art：
First, the section of the film in obtained purpose product is carried out using transmission electron microscope and X-ray diffractometer respectively
Characterize, from its result, purpose product is to invest the porous membrane with the different spherical apertures of multilayer in substrate；Wherein,
The bottom aperture of porous membrane is 1-3nm, top layer aperture is 5-8nm, and bore edges spacing is 10-2nm from bottom to top, and porosity is certainly
Upper down is 30-35% to 60-70%；This porous membrane is made up of silica.It is this by the different spherical aperture of multilayer
The purpose product that silica is assembled into, because the upper and lower surface of porous membrane is different spherical apertures and pitch of holes, that is,
With different porositys, and make purpose product that the small porosity structure of bottom can be utilized to strengthen the adhesive force with substrate, again
The hydrophily of top layer macroporosity structure can be played, and then makes purpose product while has had both wearability and Superhydrophilic.
Second, preparation method is simple, science, efficiently.The mesh of wearability and Superhydrophilic can be met simultaneously by being not only made
Product --- have graded porosity silica nanometer perforated membrane, be also prepared into the characteristics of this is relatively low, and then make
Purpose product be extremely easy to widely commercial applications in the field such as antifog, automatically cleaning, wide range be anti-reflection.
Brief description of the drawings
Fig. 1 is the section to making the film that different cetyl trimethylammonium bromide additions obtain according to preparation method
One of result characterized using transmission electron microscope (TEM).Wherein, a figures in Fig. 1 are adding for cetyl trimethylammonium bromide
The TEM image of film when dosage is 1.5wt%, by its can be seen that the spherical aperture of film be 1-2nm, bore edges spacing be 6-
7nm；B figures are the TEM image of the film when addition of cetyl trimethylammonium bromide is 4.5wt%, be can be seen that by it thin
The spherical aperture of film is 2-3nm, bore edges spacing is 3-4nm.
Embodiment
The preferred embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Bought first from market：
Tetrasilicic acid ethyl ester；
Ethanol；
Nitric acid；
Deionized water as water；
Conductor, semiconductor and insulator as substrate.
Then：
Embodiment 1
What is prepared concretely comprises the following steps：
Step 1, it is 1 according to the mol ratio of tetrasilicic acid ethyl ester, ethanol, nitric acid and water：8：0.09：3 ratio, first by four silicon
Acetoacetic ester and ethanol are mixed and stirred for, and obtain mixed solution.Nitric acid and water are mixed and stirred for again, obtain aqueous solution of nitric acid.
Step 2, first aqueous solution of nitric acid is instilled in mixed solution dropwise, and 4h is stirred at 55 DEG C；Wherein, mixing speed
For 750r/min, silicon dioxide gel is obtained.Added respectively into 3 parts of silicon dioxide gels again mass fraction for 1wt%,
3wt% and 5wt% cetyl trimethylammonium bromide, and after stirring 1h, aging 4d, obtain 3 parts of mixed sols.
Step 3, first substrate is sequentially placed into and includes cetyl trimethylammonium bromide and gradually enter in increased mixed sols
After the lifting plated film that row is 3 times, dry；Wherein, substrate be insulator in one of --- slide, lift plated film when substrate decline
Speed is 100mm/min, dip time 2min, pull rate 25mm/min, and after lifting plated film every time, it is carried out
120 DEG C, 10min drying and processing, obtain the substrate of the attached different spherical aperture perforated membranes that have three layers in surface.Have three layers again by surface is attached
The substrate of different spherical aperture perforated membranes is placed at 480 DEG C the 5h that anneals, and it is more that the silica nanometer with graded porosity is made
Pore membrane.
Embodiment 2
What is prepared concretely comprises the following steps：
Step 1, it is 1 according to the mol ratio of tetrasilicic acid ethyl ester, ethanol, nitric acid and water：8.5：0.08：3.5 ratio, first will
Tetrasilicic acid ethyl ester and ethanol are mixed and stirred for, and obtain mixed solution.Nitric acid and water are mixed and stirred for again, it is water-soluble to obtain nitric acid
Liquid.
Step 2, first aqueous solution of nitric acid is instilled in mixed solution dropwise, and 3.5h is stirred at 58 DEG C；Wherein, stirring speed
Spend for 750r/min, obtain silicon dioxide gel.Added respectively into 4 parts of silicon dioxide gels again mass fraction for 1wt%,
2wt%, 3wt% and 5wt% cetyl trimethylammonium bromide, and after stirring 1.3h, aging 4.5d, it is molten to obtain 4 parts of mixing
Glue.
Step 3, first substrate is sequentially placed into and includes cetyl trimethylammonium bromide and gradually enter in increased mixed sols
After the lifting plated film that row is 4 times, dry；Wherein, substrate be insulator in one of --- slide, lift plated film when substrate decline
Speed is 100mm/min, dip time 2min, pull rate 31mm/min, and after lifting plated film every time, it is carried out
120 DEG C, 10min drying and processing, obtain the substrate that surface has the spherical aperture perforated membrane of 4 layers of difference.Surface had 4 layers again
The substrate of different spherical aperture perforated membranes is placed at 490 DEG C the 4.5h that anneals, and the silica nanometer with graded porosity is made
Perforated membrane.
Embodiment 3
What is prepared concretely comprises the following steps：
Step 1, it is 1 according to the mol ratio of tetrasilicic acid ethyl ester, ethanol, nitric acid and water：9：0.07：4 ratio, first by four silicon
Acetoacetic ester and ethanol are mixed and stirred for, and obtain mixed solution.Nitric acid and water are mixed and stirred for again, obtain aqueous solution of nitric acid.
Step 2, first aqueous solution of nitric acid is instilled in mixed solution dropwise, and 3h is stirred at 60 DEG C；Wherein, mixing speed
For 750r/min, silicon dioxide gel is obtained.Added respectively into 5 parts of silicon dioxide gels again mass fraction for 1wt%,
2wt%, 3wt%, 4wt% and 5wt% cetyl trimethylammonium bromide, and after stirring 1.5h, aging 5d, obtain 5 parts it is mixed
Close colloidal sol.
Step 3, first substrate is sequentially placed into and includes cetyl trimethylammonium bromide and gradually enter in increased mixed sols
After the lifting plated film that row is 5 times, dry；Wherein, substrate be insulator in one of --- slide, lift plated film when substrate decline
Speed is 100mm/min, dip time 2min, pull rate 38mm/min, and after lifting plated film every time, it is carried out
120 DEG C, 10min drying and processing, obtain the substrate of the attached different spherical aperture perforated membranes that are of five storeys in surface.It is of five storeys again by surface is attached
The substrate of different spherical aperture perforated membranes is placed at 500 DEG C the 4h that anneals, and it is more that the silica nanometer with graded porosity is made
Pore membrane.
Embodiment 4
What is prepared concretely comprises the following steps：
Step 1, it is 1 according to the mol ratio of tetrasilicic acid ethyl ester, ethanol, nitric acid and water：9.5：0.06：4.5 ratio, first will
Tetrasilicic acid ethyl ester and ethanol are mixed and stirred for, and obtain mixed solution.Nitric acid and water are mixed and stirred for again, it is water-soluble to obtain nitric acid
Liquid.
Step 2, first aqueous solution of nitric acid is instilled in mixed solution dropwise, and 2.5h is stirred at 63 DEG C；Wherein, stirring speed
Spend for 750r/min, obtain silicon dioxide gel.Added respectively into 6 parts of silicon dioxide gels again mass fraction for 1wt%,
2wt%, 3wt%, 4wt%, 4.5wt% and 5wt% cetyl trimethylammonium bromide, and after stirring 1.8h, aging 5.5d,
Obtain 6 parts of mixed sols.
Step 3, first substrate is sequentially placed into and includes cetyl trimethylammonium bromide and gradually enter in increased mixed sols
After the lifting plated film that row is 6 times, dry；Wherein, substrate be insulator in one of --- slide, lift plated film when substrate decline
Speed is 100mm/min, dip time 2min, pull rate 44mm/min, and after lifting plated film every time, it is carried out
120 DEG C, 10min drying and processing, obtain the substrate that surface has the spherical aperture perforated membrane of 6 layers of difference.Surface had 6 layers again
The substrate of different spherical aperture perforated membranes is placed at 510 DEG C the 3.5h that anneals, and the silica nanometer with graded porosity is made
Perforated membrane.
Embodiment 5
What is prepared concretely comprises the following steps：
Step 1, it is 1 according to the mol ratio of tetrasilicic acid ethyl ester, ethanol, nitric acid and water：10：0.05：5 ratio, first by four
Silester and ethanol are mixed and stirred for, and obtain mixed solution.Nitric acid and water are mixed and stirred for again, obtain aqueous solution of nitric acid.
Step 2, first aqueous solution of nitric acid is instilled in mixed solution dropwise, and 2h is stirred at 65 DEG C；Wherein, mixing speed
For 750r/min, silicon dioxide gel is obtained.Added respectively into 7 parts of silicon dioxide gels again mass fraction for 1wt%,
1.5wt%, 2wt%, 3wt%, 4wt%, 4.5wt% and 5wt% cetyl trimethylammonium bromide, and after stirring 2h, always
Change 6d, obtain 7 parts of mixed sols.
Step 3, first substrate is sequentially placed into and includes cetyl trimethylammonium bromide and gradually enter in increased mixed sols
After the lifting plated film that row is 7 times, dry；Wherein, substrate be insulator in one of --- slide, lift plated film when substrate decline
Speed is 100mm/min, dip time 2min, pull rate 50mm/min, and after lifting plated film every time, it is carried out
120 DEG C, 10min drying and processing, obtain the substrate that surface has the spherical aperture perforated membrane of 7 layers of difference.Surface had 7 layers again
The substrate of different spherical aperture perforated membranes is placed at 520 DEG C the 3h that anneals, and it is more that the silica nanometer with graded porosity is made
Pore membrane.
Above-described embodiment 1-5 is repeated from the conductor or semiconductor or insulator as substrate respectively again, it is same to be made
Silica nanometer perforated membrane with graded porosity.
Obviously, those skilled in the art can be to the silica nanometer perforated membrane with graded porosity of the present invention
And preparation method thereof carry out it is various change and modification without departing from the spirit and scope of the present invention.So, if to the present invention's
These modifications and variations belong within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to include these
Including change and modification.
Claims (8)
- A kind of 1. silica nanometer perforated membrane with graded porosity, by investing the porous silica film group in substrate Into, it is characterised in that：The thickness of the porous silica film is 100-500nm, its by more than 3 layers of different spherical apertures perforated membrane group Into；The bottom aperture of more than the 3 layers different spherical aperture perforated membranes is 1-3nm, top layer aperture is 5-8nm, bore edges spacing It is 10-2nm from bottom to top, porosity is 30-35% to 60-70% from bottom to top.
- 2. the silica nanometer perforated membrane according to claim 1 with graded porosity, it is characterized in that porosity is Close porosity.
- 3. the silica nanometer perforated membrane according to claim 1 with graded porosity, it is characterized in that substrate is to lead Body, or semiconductor, or insulator.
- 4. the preparation method of the silica nanometer perforated membrane with graded porosity described in a kind of claim 1, including colloidal sol Gel method, it is characterised in that it is as follows to complete step：Step 1, it is 1 according to the mol ratio of tetrasilicic acid ethyl ester, ethanol, nitric acid and water：8-10：0.05-0.09：3-5 ratio, first Tetrasilicic acid ethyl ester and ethanol are mixed and stirred for, obtain mixed solution, then nitric acid and water are mixed and stirred for, it is water-soluble to obtain nitric acid Liquid；Step 2, first aqueous solution of nitric acid is instilled in mixed solution dropwise, and at least 2h is stirred at 55-65 DEG C, obtain titanium dioxide Ludox, then the cetyl trimethylammonium bromide that mass fraction is 1-5wt% is added into silicon dioxide gel, and stir extremely After few 1h, aging at least 4d, mixed sols is obtained；Step 3, first substrate is sequentially placed into and includes cetyl trimethylammonium bromide and gradually carry out 3 times in increased mixed sols After lifting plated film above, dry, obtain the substrate of the different spherical aperture perforated membranes of the attached above that haves three layers in surface, then surface is attached The substrate of the different spherical aperture perforated membranes of the above that haves three layers is placed at 480-520 DEG C at least 3h that anneals, and being made has graded porosity Silica nanometer perforated membrane.
- 5. the preparation method of the silica nanometer perforated membrane according to claim 4 with graded porosity, its feature It is that mixing speed when obtaining silicon dioxide gel is 750r/min.
- 6. the preparation method of the silica nanometer perforated membrane according to claim 4 with graded porosity, its feature It is that substrate is conductor, or semiconductor, or insulator.
- 7. the preparation method of the silica nanometer perforated membrane according to claim 4 with graded porosity, its feature The decrease speed for being substrate when lifting plated film is 100mm/min, dip time 2min, pull rate 25-50mm/min.
- 8. the preparation method of the silica nanometer perforated membrane according to claim 7 with graded porosity, its feature It is after each lifting plated film, 120 DEG C, 10min drying and processing is carried out to it.
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| CN108609861A (en) * | 2018-05-24 | 2018-10-02 | 沧州天瑞星光热技术有限公司 | A kind of preparation method of resistance to ultraviolet high pull rate antireflective coating |
| CN109081608A (en) * | 2018-08-22 | 2018-12-25 | 上海西源新能源技术有限公司 | Outdoor use SiO2Super 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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| 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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| US20120138215A1 (en) * | 2010-12-03 | 2012-06-07 | Samsung Electro-Mechanics Co., Ltd. | Nano glass powder for sintering additive and method for fabricating the same |
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| CN107867874B (en) | 2020-09-18 |
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