CN115117179A - Printable porous optical film and preparation method and application thereof - Google Patents
Printable porous optical film and preparation method and application thereof Download PDFInfo
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- CN115117179A CN115117179A CN202210659508.7A CN202210659508A CN115117179A CN 115117179 A CN115117179 A CN 115117179A CN 202210659508 A CN202210659508 A CN 202210659508A CN 115117179 A CN115117179 A CN 115117179A
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- 239000012788 optical film Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 239000010408 film Substances 0.000 claims abstract description 185
- 239000002002 slurry Substances 0.000 claims abstract description 87
- 239000000758 substrate Substances 0.000 claims abstract description 64
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims abstract description 44
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229940116411 terpineol Drugs 0.000 claims abstract description 44
- 229920002678 cellulose Polymers 0.000 claims abstract description 42
- 239000001913 cellulose Substances 0.000 claims abstract description 42
- 238000007650 screen-printing Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000002105 nanoparticle Substances 0.000 claims abstract description 29
- 230000003287 optical effect Effects 0.000 claims abstract description 24
- 230000001680 brushing effect Effects 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 230000001965 increasing effect Effects 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 230000007423 decrease Effects 0.000 claims abstract 3
- 239000011521 glass Substances 0.000 claims description 66
- 239000000463 material Substances 0.000 claims description 44
- 239000001856 Ethyl cellulose Substances 0.000 claims description 29
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 29
- 229920001249 ethyl cellulose Polymers 0.000 claims description 29
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 29
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 20
- 238000002834 transmittance Methods 0.000 claims description 12
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 3
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 8
- 239000002245 particle Substances 0.000 description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 26
- 239000004576 sand Substances 0.000 description 22
- 239000002994 raw material Substances 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 238000001035 drying Methods 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 9
- 239000011148 porous material Substances 0.000 description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000010409 thin film Substances 0.000 description 8
- 238000001354 calcination Methods 0.000 description 7
- 238000007639 printing Methods 0.000 description 7
- 238000002390 rotary evaporation Methods 0.000 description 7
- 238000004513 sizing Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
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- 238000003892 spreading Methods 0.000 description 4
- 230000007480 spreading Effects 0.000 description 4
- 239000013590 bulk material Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 238000002310 reflectometry Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 238000000313 electron-beam-induced deposition Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
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- 238000001228 spectrum Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
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- 239000004408 titanium dioxide Substances 0.000 description 1
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/02168—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells the coatings being antireflective or having enhancing optical properties for the solar cells
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/12—Stencil printing; Silk-screen printing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/26—Printing on other surfaces than ordinary paper
- B41M1/34—Printing on other surfaces than ordinary paper on glass or ceramic surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
Abstract
The invention discloses a printable porous optical film and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing the nano particles, cellulose and terpineol to obtain slurry, and brushing the slurry on a substrate through screen printing; heating the substrate printed with the slurry to remove cellulose in the substrate to obtain a porous optical film; the porosity of the porous optical film is changed by adjusting the content of cellulose in the slurry, and then the refractive index of the porous optical film is adjusted. The content of cellulose in the slurry is increased, the porosity of the porous optical film is increased, and the refractive index of the porous optical film is reduced; the content of cellulose in the slurry decreases, the porosity of the porous optical film decreases, and the refractive index of the porous optical film increases. The invention adopts the screen printing method to prepare the optical film, the film has better stability and optical performance, the preparation process is simple, the cost is lower, the large-scale production is easy, the refractive index of the film can be continuously adjusted in a large range, and the application range is very wide.
Description
Technical Field
The invention belongs to the field of optical films, and particularly relates to a printable porous optical film and a preparation method and application thereof.
Background
Because the spectrum and the light intensity can be regulated and controlled, the optical film has important application in various fields, such as glass windows, optical lenses, mobile phone screens, solar cells and the like. The existing optical film is generally realized by methods such as electron beam deposition, atomic layer deposition, magnetron sputtering, chemical etching, dip coater pulling (sol-gel method), thermal evaporation, spin coating, nano imprinting, self-assembly and the like, the preparation process is complex, the cost is higher, and the large-scale production is not easy to realize.
Although there are many methods and processes for preparing optical thin films, most of the optical thin films have few raw material sources, high cost and are not suitable for large-scale production due to the limitation of the processes, especially the methods and processes for preparing the optical thin films are incompatible in some fields (such as printable solar cells).
Therefore, the prior art has the technical problems of complex preparation process, higher cost and difficulty in large-scale production.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a printable porous optical film and a preparation method and application thereof, so that the technical problems of complex preparation process, higher cost and difficulty in large-scale production in the prior art are solved.
To achieve the above objects, according to one aspect of the present invention, there is provided a method of preparing a printable porous optical film, comprising:
mixing the nano particles, cellulose and terpineol to obtain slurry, and brushing the slurry on a substrate through screen printing;
heating the substrate printed with the slurry to remove cellulose in the substrate to obtain a porous optical film;
the porosity of the porous optical film is changed by adjusting the content of cellulose in the slurry, and then the refractive index of the porous optical film is adjusted.
The content of cellulose in the slurry is increased, the porosity of the porous optical film is increased, and the refractive index of the porous optical film is reduced; the content of cellulose in the slurry is reduced, the porosity of the porous optical film is reduced, and the refractive index of the porous optical film is increased.
Further, the preparation method further comprises the following steps:
by adjusting the types of the nano particles in the slurry, the refractive index of the porous optical film is adjusted on the premise of not changing the porosity of the porous optical film.
Further, the preparation method further comprises the following steps:
the thickness of the porous optical film is adjusted by changing the number of layers of paste screen-printed on the substrate or the concentration of the paste.
Further, the nano-particles are SiO 2 、ZrO 2 、TiO 2 、Ta 2 O 5 、Al 2 O 3 、ZnO、ZnS、SnO 2 、TeO 2 、Y 2 O 3 、MgO、WO 3 、MgF 2 、CeO 2 At least one of the nanoparticles.
Further, the cellulose is at least one of ethyl cellulose, hydroxypropyl cellulose and polyethylene glycol.
Further, the refractive index of the material selected for the substrate is greater than that of air, and the refractive index of the material selected for the substrate can be greater than or less than that of the porous film according to different requirements. For the preparation of the antireflection film, the refractive index of the material selected for the substrate is less than the refractive index of the porous film, and for the preparation of the antireflection film, the refractive index of the material selected for the substrate is greater than the refractive index of the porous film.
Further, the particle size of the nanoparticles is 5nm to 200nm, preferably, the particle size of the nanoparticles is 20nm to 30 nm.
Further, the mass ratio of the nanoparticles to the cellulose to the terpineol in the slurry is 1: (0.25-4): (20-140), preferably, the mass ratio of the nanoparticles to the cellulose to the terpineol in the slurry is 1: (1-2): (60-80).
According to another aspect of the present invention, there is provided a printable porous optical film, wherein the porous optical film is prepared by a method of preparing a printable porous optical film.
According to another aspect of the present invention, there is provided a use of a printable porous optical film, which is prepared by a method for preparing a printable porous optical film, wherein an optical antireflection film, an infrared filter film, an ultraviolet filter film, a light splitting film, a band-pass film in different wavelength ranges, a band-stop film in different wavelength ranges, or a polarizing film is formed by adjusting a thickness or a refractive index of the porous optical film, so as to be applied to different fields to meet different requirements.
According to another aspect of the present invention, there is provided a use of a printable porous optical film, in a solar cell, the porous optical film is prepared by a method for preparing a printable porous optical film, wherein the porosity of the porous optical film is increased by increasing the content of cellulose in the slurry, and the refractive index of the porous optical film is reduced, and the porous optical film is an optical antireflection film.
According to another aspect of the present invention, there is provided a use of a printable porous optical film, in a solar cell, the porous optical film is prepared by a method for preparing a printable porous optical film, in which a slurry is prepared by using nanoparticles having a low refractive index, the refractive index of the porous optical film is reduced without changing the porosity of the porous optical film, and the formed porous optical film is an optical antireflection film.
According to another aspect of the present invention, there is provided a use of a printable porous optical film, when used in the manufacture of light-transmitting glass,
mixing the nano particles, cellulose and terpineol to obtain slurry, and brushing the slurry on glass through screen printing;
heating the glass printed with the slurry to remove cellulose in the glass to obtain transparent glass attached with the porous optical film;
the porosity of the porous optical film is changed by adjusting the content of cellulose in the slurry, and the refractive index of the porous optical film is adjusted, so that the light transmittance of the light-transmitting glass is adjusted.
In general, compared with the prior art, the above technical solutions conceived by the present invention can achieve the following beneficial effects:
(1) according to the invention, the nano particles are used as a framework material, the cellulose is used as a pore-forming agent, the terpineol is used as a dispersion liquid, and the slurry is mixed to form the slurry, so that the slurry has good stability and can be stored for a long time, the cost of raw materials and a preparation process is low, the large-scale production of the film is easy to realize by a screen printing method, the preparation cost can be further reduced, and the preparation method can be widely applied. According to the theory of effective medium, the effective refractive index of two materials will change after mixing, and for the dielectric medium (insulating material), the effective refractive index of material C obtained by uniformly mixing materials A and B will be n C ＝p n A +(1-p)n B Wherein n is C Is the refractive index of the mixed material C, n A And n B The refractive indexes of the component materials A and B of the mixed material are respectively, and p is the volume ratio of the material A in the mixed material C. The refractive index of the nano-particles is larger than that of air, and the porous optical film is a mixed material of a framework material and air, so that the refractive index of the porous optical film is lower than that of the framework material. The refractive index of the porous material can be adjusted by adjusting the volume ratio (i.e., porosity) of air in the porous optical film, and the larger the volume ratio of air, the lower the refractive index. The preparation method of the optical film is simple, the variety of the selected materials is more, the source of the raw materials is wide, the refractive index of the film can be continuously adjusted in a large range, and the application range is wide.
(2) The invention can adjust the refractive index of the porous material by adjusting the refractive index of the framework material, and the higher the refractive index of the framework material is, the higher the refractive index of the porous material is. The refractive indices of different materials are generally different, e.g. SiO at 550nm wavelength 2 Has a refractive index of about 1.48 and is TiO 2 Has a refractive index of 2.5-2.7，ZrO 2 The refractive index of (a) is about 2.0, so that porous films prepared using different materials have different refractive indexes even in the case of the same porosity, which makes it possible to change the refractive index of the porous film by changing the raw materials for preparing the slurry to achieve a desired effect.
(3) The thickness of the film is changed by changing the concentration of the slurry, so that the film can be applied to substrates with different refractive indexes to form optical films with different functions. The content of nano particles in the unit volume of the sizing agent can be reduced by changing the mass ratio of the raw material to the terpineol, namely changing the concentration of the sizing agent, the sizing agent is used for printing and forming a film by using the same process parameters, after drying, the solvent terpineol is volatilized to form the film, the content of the nano particles in the unit volume of the film obtained by printing the sizing agent with low concentration is reduced, the film thickness of the obtained film is reduced, and the thickness of the film can be changed by adjusting the concentration of the sizing agent.
(4) According to the Fresnel formula in the optical theory,
wherein n is 0 And n 1 The refractive index of the medium on both sides of the interface, and R is the interface reflectivity. The optical reflection of the interface comes from the mismatch of the refractive indexes of the media at the two sides of the interface, so that a material with the refractive index value between the incident medium and the emergent medium is inserted between the incident medium and the emergent medium, and a certain antireflection effect can be achieved. Based on the above, the refractive index of the material selected for the substrate is larger than that of air, and the refractive index of the material selected for the substrate can be larger or smaller than that of the porous film according to different requirements.
(5) The invention can adjust the refractive index and thickness of the film by the screen printing technology, and can realize the preparation of optical films with different functions for being applied to different fields if the optical films are designed and prepared according to corresponding requirements. According to the invention, the content of cellulose in the slurry is increased, the porosity of the porous optical film is improved, the refractive index of the porous optical film is further reduced, the formed porous optical film is an optical antireflection film, and the incident light loss can be reduced by applying the optical antireflection film to the solar cell, so that the photoelectric conversion efficiency of the solar cell is effectively improved. The refractive index of the glass is about 1.52, the refractive index of air is 1, and the porous optical film printed on the glass can play a certain antireflection effect, so that the transmittance of the glass is higher.
Drawings
FIG. 1 is a schematic diagram of a printable porous optical film made according to an embodiment of the present invention;
FIG. 2 is a schematic view of a printable porous optical film provided by embodiments of the present invention;
FIG. 3 is a porous SiO solid provided in example 1 of the present invention 2 The refractive index profile of the film;
FIG. 4 is a porous SiO solid provided in example 2 of the present invention 2 The refractive index profile of the film;
FIG. 5 shows porous SiO solid provided in example 3 of the present invention 2 The refractive index profile of the film;
FIG. 6 shows porous SiO solid provided in example 4 of the present invention 2 The refractive index profile of the film;
FIG. 7 shows a porous SiO solid provided in example 5 of the present invention 2 A cross-sectional SEM photograph of the film;
FIG. 8 is a porous SiO solid provided in example 6 of the invention 2 A cross-sectional SEM photograph of the film;
FIG. 9 is a porous SiO solid provided in example 7 of the invention 2 A cross-sectional SEM photograph of the film;
FIG. 10 is a graph of printed and unprinted porous SiO provided by example 7 of the present invention 2 A graph comparing the transmittance curves of the FTO glass of the film;
FIG. 11 shows a porous TiO provided in example 8 of the present invention 2 The refractive index profile of the film;
FIG. 12 is a graph of printed and unprinted porous TiO provided in example 8 of the present invention 2 A graph comparing the transmittance curves of the FTO glass of the film;
FIG. 13 is a view showing porous ZrO provided in example 9 of the present invention 2 The refractive index profile of the film;
FIG. 14 is a graph of printed and unprinted according to example 9 of the present inventionPrinting porous ZrO 2 Transmittance curves for FTO glasses of the films are plotted against each other.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1, a method for preparing a printable porous optical film, comprising:
mixing the nano particles, cellulose and terpineol to obtain slurry, and brushing the slurry on a substrate through screen printing;
heating the substrate printed with the slurry to remove cellulose in the substrate to obtain a porous optical film;
the porosity of the porous optical film is changed by adjusting the content of cellulose in the slurry, and then the refractive index of the porous optical film is adjusted.
In fig. 1, the brush is a screen printer, and the slurry brushed on the substrate, the substrate and the platform for placing the substrate are arranged from top to bottom in sequence.
The preparation method specifically comprises the following steps:
(1) mixing the nano particles, cellulose and terpineol by a ball milling or sanding method to prepare slurry;
(2) brushing the slurry on the substrate through a screen printing machine;
(3) placing the base brushed with the sizing agent on a flat table top, flatly spreading for 1-2 hours, and then placing on a 70-80 ℃ hot table for drying (different sizing agents can be continuously printed according to different requirements);
(4) and sintering the dried film at the high temperature of 300-500 ℃ for 20-60 minutes (different according to different materials) to remove the pore-forming agent (cellulose) in the film, thereby obtaining the porous optical film.
The optical film is prepared by adopting a screen printing method, the film stability and the optical performance are good, the preparation process is simple, the cost is low, the large-scale production is easy, and the method is suitable for various fields.
Fig. 2 is a porous optical film prepared by the preparation method of the present invention, and fig. 2 is a porous optical film and a platform for placing the film in sequence from top to bottom. The porous optical film prepared by the invention is an insulating material or a semiconductor material and is not a conductor.
According to the invention, the silk-screen printing raw stock is heated to form the porous film, the raw stock consists of raw materials (nanoparticles forming the porous film, namely the aforementioned skeleton material), cellulose and terpineol, and after high-temperature sintering, the cellulose is volatilized away, so that holes are left in the film to form the porous film, and the purpose of reducing the refractive index of the material is achieved. The more cellulose content in the slurry for printing the film, the more pores are left in the film after high-temperature sintering, that is, the more air content and the larger air volume ratio in the porous material, so that the refractive index of the porous film is lower according to the formula, and therefore, the air volume ratio (porosity) in the porous film can be adjusted by adjusting the cellulose content in the slurry, thereby changing the refractive index of the film.
The preparation method of the optical film is simple, the types of the selected materials are more, the raw materials are wide in source, the refractive index of the film can be continuously adjusted in a large range (the porosity of the film is adjusted by changing the content of cellulose in the slurry so as to achieve the effect of adjusting the refractive index of the film), and the application range is extremely wide. In addition, the slurry has good stability, can be stored for a long time, has lower cost of raw materials and preparation process, is easy to realize large-scale production of films by a screen printing method, and can further reduce the preparation cost and make the films more widely applied.
The preparation method can be used for preparing the optical antireflection film, and the optical antireflection film is applied to the solar cell to reduce the loss of incident light and improve the photoelectric conversion efficiency of the solar cell.
When the preparation method is used for preparing the double-layer film, the nano particles, the cellulose and the terpineol are mixed to obtain slurry, and the slurry is brushed on a substrate through screen printing;
heating the substrate printed with the slurry to remove cellulose in the substrate to obtain a porous optical film;
two layers of slurry obtained by mixing different nano particles are sequentially brushed on a substrate to obtain a double-layer film, and the double-layer film has excellent antireflection performance and hydrophobic and self-cleaning performance.
For example, mixing TiO 2 Mixing the nanoparticles, cellulose and terpineol to obtain a first slurry, mixing SiO 2 Mixing the nano-particles, cellulose and terpineol to obtain second slurry, printing the first slurry on a substrate through screen printing, drying, continuously printing the second slurry on the substrate, drying, and then performing high-temperature annealing to remove the cellulose to prepare the TiO 2 And SiO 2 A double layer porous membrane.
Example 1
SiO with a particle size of 20nm 2 Nano SiO particles are used as raw materials 2 The particles, ethyl cellulose and terpineol are mixed according to a certain mass ratio (nano SiO) 2 Ethyl cellulose and terpineol (1: 0.25: 80) and adding proper quantity of absolute ethyl alcohol, and dispersing SiO by sand grinding method 2 The rotational speed of the sand mill is 2000rpm/h, the sanding time is 1 hour, the sanded slurry is subjected to rotary evaporation through a rotary evaporator to remove absolute ethyl alcohol, and finally, the corresponding SiO is prepared 2 The slurry was stored at room temperature.
Using FTO glass as substrate and prepared SiO 2 Preparation of SiO by Screen printing machine 2 The film is prepared by placing FTO glass substrate to be printed in the clamping groove of screen printer (glass surface facing upwards), and taking appropriate amount of SiO 2 The slurry is on the screen. The number of the adopted screen meshes is 250, and the relevant parameters of the screen printing machine are as follows: the gap between the screen plates is 1.75mm, and the pressure of the screen plates is 1.75 kg. Brushing the film on the glass surface, placing the substrate brushed with the film on a flat table for two hours after brushing so as to flatten the film as much as possible, transferring the film to a 75-DEG hot table for drying so as to remove terpineol in the film, and finally placing the dried sample in the hot table at 4 DEGCalcining at 00 ℃ for 40 minutes to remove ethyl cellulose in the film and realize pore-forming, thus obtaining SiO with mesopores (2-50nm) inside 2 A film.
According to the effective medium theory, the effective refractive index of the porous material is lower than that of the bulk material, and the porous material is considered to be a mixture of air and the bulk material, and the effective refractive index n after the mixture is f Comprises the following steps:
n f ＝p n air +(1-p)n s
wherein n is f Is porous SiO 2 Effective refractive index of the film, i.e. the refractive index measured by spectroscopic ellipsometer, n air Is refractive index of air (1), n s Is the bulk material refractive index and p is the porosity. FIG. 3 shows porous SiO obtained by printing 2 The refractive index profile of the film, n in fig. 3, represents the refractive index, which is 1.127 at 550nm, and the porosity of which is 0.747 can be calculated according to the formula.
Example 2
SiO with a particle size of 20nm 2 Nano SiO particles are used as raw materials 2 The particles, ethyl cellulose and terpineol are mixed according to a certain mass ratio (nano SiO) 2 Ethyl cellulose and terpineol (1: 0.5: 80) and adding proper quantity of absolute ethyl alcohol, and dispersing SiO by sand grinding method 2 The rotational speed of the sand mill is 2000rpm/h, the sanding time is 1 hour, the sanded slurry is subjected to rotary evaporation through a rotary evaporator to remove absolute ethyl alcohol, and finally, the corresponding SiO is prepared 2 The slurry was stored at room temperature.
Using FTO glass as substrate and prepared SiO 2 Preparation of SiO by Screen printing machine 2 The film is prepared by placing FTO glass substrate to be printed on in the clamping groove of screen printer (glass side is upward), and taking appropriate amount of SiO 2 The slurry is on the screen. The number of the adopted screen meshes is 250, and the relevant parameters of the screen printing machine are as follows: the gap between the screen plates is 1.75mm, and the pressure of the screen plates is 1.75 kg. Brushing the film on the glass surface, placing the substrate on a flat table for two hours after brushing to ensure that the film is as flat as possible, and then transferring the substrate to a 75-degree hot tableDrying to remove terpineol in the film, finally placing the dried sample in a hot bench, calcining at the high temperature of 400 ℃ for 40 minutes to remove ethyl cellulose in the film, realizing pore-forming, and obtaining SiO (silicon dioxide) with mesopores (2-50nm) in the interior 2 The refractive index profile of the film is shown in FIG. 4. Its refractive index at 550nm is 1.123 and its porosity is 0.755, which can be calculated from the formula.
Example 3
SiO with a particle size of 20nm 2 Nano SiO particles are used as raw materials 2 The particles, ethyl cellulose and terpineol are mixed according to a certain mass ratio (nano SiO) 2 Ethyl cellulose and terpineol (1: 80) in a sand mill, adding a proper amount of absolute ethyl alcohol, and dispersing SiO by using a sand mill method 2 The rotational speed of the sand mill is 2000rpm/h, the sanding time is 1 hour, the sanded slurry is subjected to rotary evaporation through a rotary evaporator to remove absolute ethyl alcohol, and finally, the corresponding SiO is prepared 2 The slurry was stored at room temperature.
Using FTO glass as substrate and prepared SiO 2 Preparation of SiO by Screen printing machine 2 The film is prepared by placing FTO glass substrate to be printed in the clamping groove of screen printer (glass surface facing upwards), and taking appropriate amount of SiO 2 The slurry is on the screen. The number of the adopted screen meshes is 250, and the relevant parameters of the screen printing machine are as follows: the gap between the screen plates is 1.75mm, and the pressure of the screen plates is 1.75 kg. Brushing the film on a glass surface, after brushing, placing the substrate brushed with the film on a flat table for two hours to flatten the film as much as possible, then transferring the film to a 75-DEG C hot table for drying to remove terpineol in the film, finally placing the dried sample in the hot table, calcining at the high temperature of 400 ℃ for 40 minutes to remove ethyl cellulose in the film, realizing pore-forming, and obtaining SiO and the film containing mesopores (2-50nm) inside. The refractive index curve is shown in fig. 5, the refractive index at 550nm is 1.140, and the porosity is 0.720 according to the formula.
Example 4
SiO with a particle size of 20nm 2 Nano SiO particles are used as raw materials 2 The particles, ethyl cellulose and terpineol are mixed according to a certain mass ratio (nano SiO) 2 Ethyl cellulose and terpineol (1: 2: 80) in a sand mill, adding a proper amount of absolute ethyl alcohol, and dispersing SiO by using a sand mill method 2 The rotational speed of the sand mill is 2000rpm/h, the sanding time is 1 hour, the sanded slurry is subjected to rotary evaporation through a rotary evaporator to remove absolute ethyl alcohol, and finally, the corresponding SiO is prepared 2 The slurry was stored at room temperature.
Using FTO glass as substrate and prepared SiO 2 Preparation of SiO by Screen printing machine 2 The film is prepared by placing FTO glass substrate to be printed in the clamping groove of screen printer (glass surface facing upwards), and taking appropriate amount of SiO 2 The slurry is on the screen. The number of the adopted screen meshes is 250, and the relevant parameters of the screen printing machine are as follows: the gap between the screen plates is 1.75mm, and the pressure of the screen plates is 1.75 kg. Brushing a film on a glass surface, placing the substrate on which the film is brushed on a flat table for flatly spreading for two hours after brushing, flatly spreading the film as much as possible, transferring the film to a hot table at 75 ℃ for drying to remove terpineol in the film, placing a dried sample in the hot table, calcining at the high temperature of 400 ℃ for 40 minutes to remove ethyl cellulose in the film, realizing pore-forming, and obtaining SiO (silicon dioxide) with mesopores (2-50nm) in the film 2 A film. The refractive index curve is shown in FIG. 6, the refractive index at 550nm is 1.140, and the porosity is 0.720 according to the formula.
Example 5
SiO with a particle size of 20nm 2 Nano SiO particles are used as raw materials 2 The particles, the ethyl cellulose and the terpineol are respectively mixed according to three mass ratios (nanometer SiO) 2 Ethyl cellulose and terpineol in the ratio of 1 to 60) are added into a sand mill, then a proper amount of absolute ethyl alcohol is added, and SiO is dispersed by a sand milling method 2 The rotation speed of the sand mill is 2000rpm/h, the sanding time is 1 hour, the sanded slurry is subjected to rotary evaporation through a rotary evaporator to remove absolute ethyl alcohol, and finally, the corresponding SiO is prepared 2 The slurry was stored at room temperature.
Using FTO glass as substrate and prepared SiO 2 Passing of the slurryPreparation of SiO by screen printing machine 2 The film is prepared by placing FTO glass substrate to be printed in the clamping groove of screen printer (glass surface facing upwards), and taking appropriate amount of SiO 2 The slurry is on the screen. The number of the adopted screen meshes is 250, and the relevant parameters of the screen printing machine are as follows: the gap between the screen plates is 1.75mm, and the pressure of the screen plates is 1.75 kg. Brushing a film on a glass surface, after brushing, placing a substrate brushed with the film on a flat table for two hours to flatten the film as much as possible, then transferring the film to a 75-DEG C hot table for drying to remove terpineol in the film, finally placing a dried sample in the hot table, calcining at the high temperature of 400 ℃ for 40 minutes to remove ethyl cellulose in the film, realizing pore-forming, and obtaining porous SiO with the inside containing mesopores (2-50nm) and the thickness of about 320nm 2 The film is shown in FIG. 7 in a SEM photograph of a cross section.
Example 6
SiO with a particle size of 20nm 2 Nano SiO particles are used as raw materials 2 The particles, the ethyl cellulose and the terpineol are respectively mixed according to three mass ratios (nanometer SiO) 2 Ethyl cellulose and terpineol (1: 80) in a sand mill, adding a proper amount of absolute ethyl alcohol, and dispersing SiO by using a sand mill method 2 The rotational speed of the sand mill is 2000rpm/h, the sanding time is 1 hour, the sanded slurry is subjected to rotary evaporation through a rotary evaporator to remove absolute ethyl alcohol, and finally, the corresponding SiO is prepared 2 The slurry was stored at room temperature.
Using FTO glass as substrate and prepared SiO 2 Preparation of SiO by Screen printing machine 2 The film is prepared by placing FTO glass substrate to be printed in the clamping groove of screen printer (glass surface facing upwards), and taking appropriate amount of SiO 2 The slurry is on the screen. The number of the adopted screen meshes is 250, and the relevant parameters of the screen printing machine are as follows: the gap between the screen plates is 1.75mm, and the pressure of the screen plates is 1.75 kg. Brushing the film on the glass surface, placing the substrate brushed with the film on a flat table for two hours after brushing so as to flatten the film as much as possible, transferring the film to a 75-DEG hot table for drying so as to remove terpineol in the film, and finally placing the dried sample on the glass surfaceCalcining at 400 deg.C for 40 min to remove ethyl cellulose in the film and form pores, and obtaining porous SiO with thickness of 240nm and mesopores (2-50nm) 2 A SEM (scanning Electron microscope) photograph of the cross section of the thin film is shown in FIG. 8.
Example 7
SiO with a particle size of 20nm 2 Nano SiO particles are used as raw materials 2 The particles, the ethyl cellulose and the terpineol are respectively mixed according to three mass ratios (nanometer SiO) 2 Ethyl cellulose and terpineol in the ratio of 1 to 60) are added into a sand mill, then a proper amount of absolute ethyl alcohol is added, and SiO is dispersed by a sand milling method 2 The rotational speed of the sand mill is 2000rpm/h, the sanding time is 1 hour, the sanded slurry is subjected to rotary evaporation through a rotary evaporator to remove absolute ethyl alcohol, and finally, the corresponding SiO is prepared 2 The slurry was stored at room temperature.
Using FTO glass as substrate and prepared SiO 2 Preparation of SiO by Screen printing machine 2 The film is prepared by placing FTO glass substrate to be printed in the clamping groove of screen printer (glass surface facing upwards), and taking appropriate amount of SiO 2 The slurry is on the screen. The number of the adopted screen meshes is 250, and the relevant parameters of the screen printing machine are as follows: the gap between the screen plates is 1.75mm, and the pressure of the screen plates is 1.75 kg. Brushing a film on a glass surface, after brushing, placing a substrate brushed with the film on a flat table for spreading for two hours to flatten the film as much as possible, then transferring the film to a 75-DEG C hot table for drying to remove terpineol in the film, finally placing a dried sample in the hot table, calcining at the high temperature of 400 ℃ for 40 minutes to remove ethyl cellulose in the film, realizing pore-forming, and obtaining porous SiO with the inside containing mesopores (2-50nm) and the thickness of about 180nm 2 The film is shown in FIG. 9 in a SEM photograph of a cross section.
According to the Fresnel formula in the optical theory,
wherein n is 0 And n 1 The refractive index of the medium on both sides of the interface, and R is the interface reflectivity. Interface (I)The optical reflection of the light source is from the mismatch of the refractive indexes of the media at the two sides of the interface, so that a material with the refractive index value between the incident medium and the emergent medium is inserted between the incident medium and the emergent medium, and a certain antireflection effect can be achieved. The refractive index of the glass is about 1.52, the refractive index of the air is 1, and porous SiO is printed on the glass surface of the FTO glass 2 The optical film can play a certain role in antireflection, so that the transmittance of the optical film is higher, and the SiO film in the embodiment is printed 2 Optical film and unprinted SiO 2 The transmittance curve of FTO glass for optical films is shown in FIG. 10, and it is evident that porous SiO is printed on the film 2 After the film is formed, the transmittance of the FTO glass is improved, and the maximum transmittance is improved from 85 percent to 89 percent.
Example 8
As purchased TiO of 30nm particle size 2 Virgin pulp as raw material, TiO 2 The raw pulp contains ethyl cellulose, and a certain amount of TiO is taken 2 Virgin pulp and terpineol, TiO 2 The mass ratio of the primary pulp to the terpineol is 1: 4 (the proportion is adjustable), then the primary pulp and the terpineol are put in an ultrasonic machine for ultrasonic treatment for 48 hours to be uniformly mixed, and finally TiO is obtained 2 The slurry was stored at room temperature.
Using FTO glass as substrate and prepared TiO 2 Preparation of TiO from the slurry by Screen printing 2 The film is prepared by placing FTO glass substrate to be printed in the clamping groove of screen printer (FTO side is upward), and taking appropriate amount of TiO 2 The slurry is on the screen. The adopted screen mesh number is 150, and the relevant parameters of the screen printing machine are as follows: the gap between the screen plates is 1.75mm, and the pressure of the screen plates is 1.75 kg. Brushing a film on an FTO surface, after brushing, placing a substrate brushed with the film on a flat table for two hours to flatten the film as much as possible, then transferring the film to a 75-DEG C hot table for drying to remove terpineol in the film, finally placing a dried sample in the hot table, calcining at a high temperature of 500 ℃ for 40 minutes to remove ethyl cellulose in the film, realizing pore-forming, and obtaining TiO (titanium dioxide) with mesopores (2-50nm) in the interior 2 The refractive index profile of the film is shown in FIG. 11. At 550nm, its refractive index value is 1.40, which is better than the original TiO 2 Is lower (2.5-2.7), indicating thatMesoporous pores successfully reduced their refractive index. The porous TiO is mixed with 2 The film is printed on the glass surface of the FTO glass, so that the transmittance of the FTO glass is successfully improved, and a certain antireflection effect is achieved, as shown in figure 12.
Example 9
ZrO with a particle size of 30nm 2 Nano-sized ZrO is prepared from nano-sized particles 2 The particles, ethyl cellulose and terpineol are mixed according to a certain mass ratio (nano ZrO) 2 Adding ethyl cellulose and terpineol (1: 0.5: 80) into a sand mill, adding a proper amount of glacial acetic acid (for adjusting the dispersion of the slurry) and a proper amount of absolute ethyl alcohol, and dispersing ZrO by using a sand mill 2 The rotational speed of the sand mill is 2300rpm/h, the sanding time is 30 minutes, the slurry obtained after sanding is steamed by a rotary steaming instrument to remove the absolute ethyl alcohol, and finally, the corresponding ZrO is obtained by preparation 2 The slurry was stored at room temperature.
Preparing ZrO by using FTO glass as a substrate 2 Preparation of ZrO from the paste by means of a Screen printing machine 2 The film is prepared by placing FTO glass substrate to be printed in the clamping groove of screen printer (glass side is upward), and taking appropriate amount of ZrO 2 The slurry is on the screen. The number of the adopted screen meshes is 250, and the relevant parameters of the screen printing machine are as follows: the screen gap is 1.75mm, and the screen pressure is 1.75kg (the parameters of the screen printing machine can be adjusted). After printing by a screen printer, placing the FTO glass substrate with the film on a flat table for two hours to flatten the film as much as possible, then transferring the FTO glass substrate to a 75-DEG C hot table for drying to remove terpineol in the film, finally placing a dried sample in the hot table, calcining at the high temperature of 400 ℃ for 40 minutes to remove ethyl cellulose in the film, realizing pore-forming, and obtaining ZrO with mesopores (2-50nm) inside 2 The refractive index profile of the film is shown in FIG. 13. At 550nm, the value of the refractive index is 1.23, which is larger than the original ZrO 2 Is lower (2.0-2.2), indicating that pore-formation successfully reduced its refractive index. The porous TiO is mixed with 2 The film is printed on the glass surface of the FTO glass, so that the transmittance of the FTO glass is successfully improved, and a certain antireflection effect is achieved, as shown in fig. 14.
In the above embodiments, the slurry can be prepared by other materials to obtain optical antireflection films of different raw materials, such as Ta 2 O 5 、Al 2 O 3 、ZnO、ZnS、SnO 2 、TeO 2 、Y 2 O 3 、MgO、WO 3 、MgF 2 、CeO 2 And the like. The particle size is not limited to 20nm and 30nm, the thickness of the film can be adjusted by changing the concentration of the slurry, and the refractive index of the film can be adjusted by changing the mass ratio of the raw material to the ethyl cellulose in the slurry. The film can be deposited together in multiple layers to form an optical film with better performance and wider functions, and the sintering of the film can be carried out once every deposited layer, or the film can be sintered together after multiple layers (two or more layers) of films are deposited. Through the combination of different types of films, optical films with multiple purposes can be formed, such as optical antireflection films, infrared filter films, ultraviolet filter films, light splitting films, band-pass or band-stop films with different wavelength ranges, polarizing films and the like, so as to meet different requirements in different fields.
According to the optical theory, the optical thin film with different functions can be obtained by adjusting the refractive index and the thickness of the thin film and the stacking mode between the thin films. For the antireflection film, as long as a thin film with the refractive index between the substrate material and the incident medium is deposited on the substrate, the transition of the refractive index between the incident medium and the substrate can be realized, the reflection of an interface is reduced, and the antireflection effect is achieved. According to the wave optics theory, when the optical path difference of two beams of light (with the same frequency) is odd times and even times of 1/4 wavelengths, destructive interference and constructive interference can be satisfied respectively, and the antireflection and reflection increasing effects can be achieved, so that the antireflection and reflection increasing performances can be achieved respectively by adjusting the thickness of the printed optical film. For the basic configuration of
Wherein H is a high refractive index material, the film thickness is λ/4, H/2 represents the film thickness of λ/8, L is a low refractive index material, the film thickness is λ/4, λ is a reference center wavelength and is also a center wavelength of the cut-off band, and m is a periodic period of the film systemAnd (4) counting. The long-wave-pass filter film can filter light with shorter wavelength to form a long-wave-pass filter film. The high-refractive-index material and the low-refractive-index material are alternately deposited by a screen printing technology, the thicknesses of the high-refractive-index material and the low-refractive-index material are respectively selected to be 1/8 and 1/4 of the reference wavelength, the preparation of the long-wave-pass filter film can be realized, the position of the center wavelength of the long-wave-pass filter film is adjusted, the wavelength range which the long-wave-pass filter film penetrates through can fall in an infrared light area, and the infrared filter film is prepared. On the contrary, for the basic configuration
The film system can filter photons with long wavelength to form a short-wavelength-pass filter film. Similarly, a low refractive index material and a high refractive index material with the thicknesses of 1/8 wavelengths and 1/4 wavelengths are alternately deposited by a screen printing technology, so that a short-wavelength-pass filter film can be realized, the position of the reference wavelength is adjusted, the transmitted wavelength range falls in an ultraviolet region, and the ultraviolet filter film is formed. The band-pass or band-stop filter film can be realized by combining the short-wave-pass filter film and the long-wave-pass filter film, and the band-pass or band-stop in a desired range can be realized by adjusting the position of the reference center wavelength. The band-pass filter film can also be basically configured as LHL m Wherein L and H represent a low refractive index material and a high refractive index material, respectively, having a thickness of 1/4 wavelengths, a bandpass in a desired wavelength range can be achieved by adjusting the position of the reference center wavelength. Therefore, the band-pass filter film can be prepared by depositing materials with high refractive index and low refractive index alternately by a screen printing technology. In short, the refractive index and thickness of the film can be adjusted by the screen printing technique, and thus if the optical film is designed and manufactured according to the corresponding requirements, the optical film with different functions can be manufactured to be applied to different fields.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A method of making a printable porous optical film, comprising:
mixing the nano particles, cellulose and terpineol to obtain slurry, and brushing the slurry on a substrate through screen printing;
heating the substrate printed with the slurry to remove cellulose in the substrate to obtain a porous optical film;
the porosity of the porous optical film is changed by adjusting the content of cellulose in the slurry, and then the refractive index of the porous optical film is adjusted.
2. The method of claim 1, wherein the method further comprises:
by adjusting the types of the nano particles in the slurry, the refractive index of the porous optical film is adjusted on the premise of not changing the porosity of the porous optical film.
3. The method of claim 1 or 2, wherein the method further comprises:
the thickness of the porous optical film is adjusted by changing the number of layers of paste screen-printed on the substrate or the concentration of the paste.
4. The method of claim 1 or 2, wherein the nanoparticles are SiO 2 、ZrO 2 、TiO 2 、Ta 2 O 5 、Al 2 O 3 、ZnO、ZnS、SnO 2 、TeO 2 、Y 2 O 3 、MgO、WO 3 、MgF 2 、CeO 2 At least one of the nanoparticles.
5. The method of claim 1 or 2, wherein the cellulose is at least one of ethyl cellulose, hydroxypropyl cellulose and polyethylene glycol.
6. The method of claim 1 or 2, wherein the substrate is made of a material having a refractive index greater than the refractive index of air.
7. A printable porous optical film prepared by the method of any one of claims 1-6.
8. The application of a printable porous optical film, wherein the porous optical film is prepared by the method for preparing a printable porous optical film according to any one of claims 1 to 6, and during preparation, an optical antireflection film, an infrared filter film, an ultraviolet filter film, a light splitting film, band-pass films in different wavelength ranges, band-stop films in different wavelength ranges or a polarizing film is formed by adjusting the thickness or the refractive index of the porous optical film, so that the application in different fields can meet different requirements.
9. Use of a printable porous optical film in a solar cell, wherein the porous optical film is prepared by the method of any one of claims 1 to 6, and the method comprises increasing the cellulose content in the slurry to increase the porosity of the porous optical film and further decrease the refractive index of the porous optical film, and the porous optical film is an optical antireflection film.
10. The application of a printable porous optical film is characterized in that when the porous optical film is applied to the preparation of light-transmitting glass,
mixing the nano particles, cellulose and terpineol to obtain slurry, and brushing the slurry on glass through screen printing;
heating the glass printed with the slurry to remove cellulose in the glass to obtain light-transmitting glass attached with the porous optical film;
the porosity of the porous optical film is changed by adjusting the content of cellulose in the slurry, and the refractive index of the porous optical film is adjusted, so that the light transmittance of the light-transmitting glass is adjusted.
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