CN114525003A - Optical film and preparation method thereof - Google Patents

Optical film and preparation method thereof Download PDF

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Publication number
CN114525003A
CN114525003A CN202210176574.9A CN202210176574A CN114525003A CN 114525003 A CN114525003 A CN 114525003A CN 202210176574 A CN202210176574 A CN 202210176574A CN 114525003 A CN114525003 A CN 114525003A
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solution
ethyl alcohol
silica
absolute ethyl
silicon dioxide
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迟聪聪
张丹洁
线佳荣
许馨
屈盼盼
张素风
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2339/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
    • C08J2339/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
    • C08J2339/06—Homopolymers or copolymers of N-vinyl-pyrrolidones
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/16—Solid spheres
    • C08K7/18—Solid spheres inorganic

Abstract

The invention discloses an optical film and a preparation method thereof, the method has the advantages of easily obtained raw materials, simple process, low price and easy mass production, and ethyl orthosilicate is used as a silicon source, absolute ethyl alcohol is used as a solvent, and ammonia water is used as a catalyst to generate silicon dioxide particles with better monodispersity. The whole preparation method is mild in reaction condition and easy to control, and the silicon dioxide microspheres with the particle size having the normal distribution characteristic can be controllably prepared by adopting a precursor multi-step dropping method. The solution of blending PVA aqueous solution, PVP aqueous solution and silica suspension is adopted for pouring self-assembly film formation, so that the dispersibility of the silica microspheres in the water phase and the uniformity, transparency and strength of the silica film formation are enhanced, and the color effect of the structural color of the silica-based optical film is enhanced.

Description

Optical film and preparation method thereof
Technical Field
The invention belongs to the field of preparation of functional film materials, and particularly relates to an optical film and a preparation method thereof.
Background
The film material has a special shape, and is deposited or condensed on the surface of the substrate into a special substance layer by adopting a special process or method, so that the film material has unique optical, electrical, chemical and other characteristics different from those of the bulk material. With the rapid development of electronic information technology, the development of microelectronic and solid electronic technologies is also changing day by day, thereby promoting the wide application of thin film materials in different fields. The structural color is an optical effect generated by the self structural characteristic of an object on a sub-microstructure, and has the characteristics of bright color, high saturation, cleanness, environmental protection, fastness, controllable color and the like. In recent years, structural color film materials are increasingly used in the fields of electronic devices, optical devices, printing and packaging materials and the like. The silicon dioxide-based structural color film is widely researched and applied due to the fact that raw materials are easy to obtain and the process is simple, but the problems of poor dispersity, poor film forming color and the like exist when silicon dioxide microspheres are self-assembled into the structural color film in a water phase.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an optical film and a preparation method thereof, and provides a thought for ensuring that the silicon dioxide microspheres are dispersed more uniformly and the film forming color is brighter when the silicon dioxide microspheres are formed into a film in a water phase.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a method of making an optical film comprising the steps of:
step 1, mixing absolute ethyl alcohol, water and ammonia water, and then dropwise adding tetraethoxysilane for reaction to generate a seed solution A;
step 2, mixing absolute ethyl alcohol, water and ammonia water, and adding the seed solution A to generate a reaction solution B;
step 3, adding tetraethoxysilane and the mixed solution C into the reaction solution B, and reacting to generate a solution D; the adding amount of the tetraethoxysilane and the mixed solution C is equal; the mixed solution C is a mixture of ammonia water, water and absolute ethyl alcohol;
step 4, purifying the solution D, drying and grinding the purified product to obtain silicon dioxide microspheres;
step 5, preparing a silicon dioxide suspension through silicon dioxide microspheres, and adding a PVA (polyvinyl acetate) aqueous solution and a PVP (polyvinyl pyrrolidone) aqueous solution into the silicon dioxide suspension to obtain a blending solution E;
and step 6, obtaining the optical film with the silicon dioxide-based structural color by blending the solution E.
The invention is further improved in that:
preferably, in the step 1, the mixing volume ratio of the absolute ethyl alcohol, the water and the ammonia water is (150-: (23-33): (4-8);
the reaction temperature is 60-65 ℃, and the reaction time is 10-12 h.
Preferably, in the step 2, the mixing volume ratio of the absolute ethyl alcohol, the water and the ammonia water is (150-: (26-32): (26-32).
Preferably, in step 2, the mixing volume ratio of the seed solution a to the absolute ethyl alcohol is: (4-8):
(150-160)。
preferably, in the step 3, the mixing ratio of the tetraethoxysilane to the seed solution in the step 2 is (17-23): (4-8);
in the step 3, the volume ratio of the ammonia water to the absolute ethyl alcohol in the mixed solution C is 7:3: 10.
Preferably, in the step 3, the reaction temperature is 25-35 ℃ and the reaction time is 4-5 h.
Preferably, in the step 4, the drying temperature is 40-45 ℃ and the drying time is 6-10 h.
Preferably, in step 5, the mass fraction of the silica microspheres in the silica suspension is 0.3% -0.6%.
Preferably, in step 5, the mass ratio of the PVP aqueous solution in the blending solution E is 0.7-2.5%, and the mass ratio of the silica suspension to the PVA aqueous solution is (0.5-2.0): (0.5-1.5).
The optical film is formed by pouring and self-assembling a blended solution, wherein the blended solution contains silica microspheres, and the particle size of the silica microspheres is 200-750 nm.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of an optical film, which has the advantages of easily obtained raw materials, simple process, low price and easy mass production, and takes tetraethoxysilane as a silicon source, absolute ethyl alcohol as a solvent and ammonia water as a catalyst to generate silicon dioxide particles with better monodispersity. Preparing a silica suspension solution with a certain mass fraction, adding a PVA aqueous solution and a PVP aqueous solution with a certain mass fraction, blending, and pouring the self-assembly in a culture dish or on a glass sheet to generate the silica-based photonic crystal structure color film. The whole preparation method is mild in reaction condition and easy to control, and the silicon dioxide microspheres with the particle size having the normal distribution characteristic can be controllably prepared by adopting a precursor multi-step dropping method. The solution of blending PVA aqueous solution, PVP aqueous solution and silica suspension is adopted for pouring self-assembly film formation, so that the dispersibility of the silica microspheres in the water phase and the uniformity, transparency and strength of the silica film formation are enhanced, and the color effect of the structural color of the silica-based optical film is enhanced.
The invention also discloses an optical film, which is prepared by blending, pouring and self-assembling the silica microsphere suspension, the PVA aqueous solution and the PVP aqueous solution in a culture dish or on a glass sheet. Has wide application prospect in the fields of printing packaging materials, microelectronic devices, optical devices and the like.
The invention discloses an optical film, which has the advantages of easily obtained raw materials, simple process, low price and easy mass production. The silicon dioxide particles with the particle size of 200-750nm are prepared by taking tetraethoxysilane as a silicon source, absolute ethyl alcohol as a solvent and ammonia water as a catalyst. Preparing a silica suspension solution with a certain mass fraction, adding a PVA aqueous solution and a PVP aqueous solution with a certain mass fraction, blending, and self-assembling in a culture dish or on a glass sheet to generate the silica-based photonic crystal structure color film. The self-assembly film forming is carried out by adopting the blending solution of the PVA aqueous solution, the PVP aqueous solution and the silica suspension, the dispersibility of the silica microspheres in the aqueous phase and the uniformity, transparency and strength of the silica film forming are enhanced, and the color effect of the structural color of the silica-based optical film is enhanced.
Drawings
FIG. 1 is a view of the observation of self-assembled silica photonic crystals on a glass slide under a point light source in example 1 of the present invention.
Fig. 2 is a color development effect graph of an iridescent film prepared in example 5 of the present invention.
Fig. 3 is a surface 3D effect plot of an iridescent film prepared in example 5 of the present invention.
Fig. 4 is a graph of the light transmission of iridescent films prepared in examples 3-6 of the present invention.
Fig. 5 is a color development effect graph of an iridescent film prepared in example 8 of the present invention.
Fig. 6 is a surface 3D effect plot of an iridescent film prepared in example 9 of the present invention.
Fig. 7 is a surface 3D effect plot of an iridescent film prepared in example 10 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
the invention is further described in detail with reference to the following drawings and examples, and discloses a preparation method of an optical film, which specifically comprises the following steps:
(1) adding 160mL of anhydrous ethanol, 23-33mL of deionized water and 4-8mL of ammonia water into the three-mouth bottle; 4-8mL of tetraethyl orthosilicate (TEOS) is added dropwise, the reaction temperature is 60-65 ℃, the reaction duration is 10-12h, and after TEOS hydrolysis and condensation reaction, a seed solution A is formed. In this step, some silica microspheres having a particle size are generated in the seed solution a, so that these preliminarily formed silica microspheres can be used in the next step.
(2) Adding 160mL of absolute ethyl alcohol 150-.
(3) Slowly dropwise adding equal amounts of TEOS solution and ammonia water/H into the reaction solution B formed in the step (2)2O/absolute ethyl alcohol mixed solution C (the volume ratio of each component in the solution C is ammonia water: H)2O anhydrous ethanol ═ 7:3:10), the TEOS solution and ammonia/H2The dropwise adding amount of the O/absolute ethyl alcohol mixed solution C is 17-23mL, the synthesis rate of silicon dioxide is controlled by a bidirectional dropwise adding reagent, so that the particle size range of the prepared silicon dioxide microspheres is large, and the bidirectional dropwise adding reagent is a TEOS solution and ammonia water/H2The O/absolute ethyl alcohol mixed solution C, the solution B and the bidirectional dropwise adding reagent react for 4-5 hours at the temperature of 25-35 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, drying the centrifugal product at the temperature of 40-45 ℃ for 6-10h, and fully grinding to obtain the silicon dioxide microspheres. The method can prepare the silica microspheres with multiple particle sizes at one time, and the particle size of the silica microspheres is between 200 and 750 nm.
(5) Preparing a suspension with the mass fraction of 0.3% -0.6% in water by using the silica microspheres obtained in the step (4), adding a PVA aqueous solution with the mass fraction of 8% and a PVP aqueous solution with the mass fraction of 5% to react to obtain a blended solution E, wherein the mass percentage of the added PVP aqueous solution in the blended solution E is 0.7% -2.5%, and the mass ratio of the silica suspension to the PVA aqueous solution in the mixed solution is (0.5-2.0): (0.5-1.5).
(6) Pouring the blending solution E prepared in the step (5) into a culture dish or dripping the blending solution E on a glass sheet to self-assemble to obtain the silica-based structural color optical film.
Example 1
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 60 ℃ and the reaction time was 10h, and a solution A was formed after the reaction.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of solution A obtained in the step (1), and then addingSiO in continuous stirring regulating system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)220mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 5h at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). And self-assembling to form the silicon dioxide photonic crystal on a clean glass sheet substrate.
FIG. 1 is a view of the self-assembled silica photonic crystal of this example viewed under a point light source on a glass slide. As can be seen from the figure, the photonic crystal film has gorgeous structural color, and the feasibility of forming the photonic crystal by self-assembly is verified.
Example 2
(1) 155mL of absolute ethyl alcohol, 30mL of deionized water and 4mL of ammonia water are added into a three-mouth bottle; 4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 65 ℃ and the reaction time was 10h, and a solution A was formed after the reaction was completed.
(2) Adding 155mL of absolute ethyl alcohol, 30mL of deionized water and 27mL of ammonia water into a three-necked bottle, stirring at a low rotating speed, adding 4.2 mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)2And (3) respectively preparing 22mL of O/absolute ethyl alcohol/ammonia water mixed solution C, controlling the synthesis rate of silicon dioxide bidirectionally, and reacting for 5 hours at 27 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 8 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). 0.5g of a 0.3% silica solution was mixed with 1.5g of 8% PVA aqueous solution to obtain solution E.
(6) And (3) pouring the solution E obtained in the step (5) into a culture dish or dripping the solution E on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 3
(1) 160mL of absolute ethyl alcohol, 26mL of deionized water and 5mL of ammonia water are added into a three-mouth bottle; 5mL of tetraethyl orthosilicate (TEOS) is slowly added, the reaction temperature is 60 ℃, the reaction time is 11h, and a solution A is formed after the reaction is finished.
(2) Adding 160mL of absolute ethyl alcohol, 32mL of deionized water and 30mL of ammonia water into a three-necked bottle, stirring at a low rotating speed, adding 4.5mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)2And (3) respectively preparing 22mL of O/absolute ethyl alcohol/ammonia water mixed solution C, controlling the synthesis rate of silicon dioxide bidirectionally, and reacting for 4h at the temperature of 30 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 10 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.4% by using the silicon dioxide obtained in the step (4). 0.5g of a 0.4% silica solution was mixed with 1.0g of an 8% PVA aqueous solution to obtain a solution E.
(6) And (3) pouring the solution E obtained in the step (5) into a culture dish or dripping the solution E on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 4
(1) Adding 150mL of absolute ethyl alcohol, 23mL of deionized water and 4mL of ammonia water into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 65 ℃ and the reaction time was 10h, and a solution A was formed after the reaction.
(2) Adding 150mL of absolute ethyl alcohol, 26mL of deionized water and 26mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)2O/absolute ethyl alcohol/ammonia waterThe mixed solution C of (1) was 21mL each, and the silica synthesis rate was controlled bidirectionally, and reacted at 26 ℃ for 5 hours to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 10 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). 0.5g of a 0.3% silica solution was mixed with 0.5g of 8% PVA aqueous solution to obtain solution E.
(6) And (3) pouring the solution E obtained in the step (5) into a culture dish or dripping the solution E on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 5
(1) Adding 155mL of absolute ethyl alcohol, 28mL of deionized water and 5mL of ammonia water into a three-necked bottle; 4.5mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 60 ℃ and the reaction time was 11h, and a solution A was formed after the reaction was completed.
(2) Adding 155mL of absolute ethyl alcohol, 32mL of deionized water and 30mL of ammonia water into a three-necked bottle, stirring at a low rotating speed, adding 4.4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)219mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 5h at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying for 7 hours at the temperature of 45 ℃ to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). 1.0g of a 0.3% silica solution was mixed with 0.5g of 8% PVA aqueous solution to obtain solution E.
(6) And (4) pouring the solution E obtained in the step (5) into a culture dish or dripping the solution E on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Fig. 2 is a color development effect diagram of the silica/PVA iridescent film prepared in this example under a point light source, and the structural color of the iridescent film can be observed more clearly, but the iridescent film is not bright due to non-uniform film formation and a whitening phenomenon.
Fig. 3 is a 3D effect diagram of the surface of the iridescent film prepared in this embodiment, and it can be seen that there are many raised portions on the surface of the iridescent film, which indicates that the surface of the film is extremely uneven and the uniformity of the formed film is relatively general.
Example 6
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 65 ℃ and the reaction time was 11h, and a solution A was formed after the reaction was completed.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)220mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 4h at 28 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying for 8 hours at the temperature of 45 ℃ to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.4% by using the silicon dioxide obtained in the step (4). 1.5g of a 0.4% silica solution was mixed with 0.5g of 8% PVA aqueous solution to obtain solution E.
(6) And (3) pouring the solution E obtained in the step (5) into a culture dish or dripping the solution E on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
FIG. 4 is SiO as described in examples 3 to 62Transmittance profile of iridescent films prepared from different mass ratios of suspension to PVA aqueous solution. As can be seen from the figure, the highest transmittance of the iridescent film in example 3 and the lowest transmittance of the iridescent film in example 6 indicate that the change in the mass fraction of the silica suspension significantly changes the transmittance of the iridescent film, thereby affecting the color development effect.
Example 7
(1) 160mL of absolute ethyl alcohol, 28mL of deionized water and 5mL of ammonia water are added into a three-mouth bottle; 4.6mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 60 ℃ and the reaction time was 10h, and a solution A was formed after the reaction.
(2) Adding 160mL of absolute ethyl alcohol, 32mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)2The O/absolute ethyl alcohol/ammonia water mixed solution C is 18mL respectively, the synthesis rate of silicon dioxide is controlled bidirectionally, and the reaction is carried out for 5h at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 45 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). Solution E was obtained by mixing 2.0g of a 0.3% silica solution with 0.5g of 8% PVA solution in water.
(6) And (3) pouring the solution E obtained in the step (5) into a culture dish or dripping the solution E on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 8
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 60 ℃ and the reaction time was 10h, and a solution A was formed after the reaction.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)220mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 5h at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). A mixed solution E of 1.0g of a 0.3% silica solution and 0.5g of an 8% PVA aqueous solution was mixed with a PVP aqueous solution of 2.5% by mass in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Fig. 5 is a graph of the color development effect of the iridescent film prepared in this example. Compared with a silica/PVA iridescent film without PVP (shown in figure 2), the iridescent film with PVP is more bright in color and smoother and uniform in formed film, namely, the dispersibility of the silica microspheres is improved by the PVP.
Example 9
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was added slowly at 60 ℃ for 10h to form solution A after the reaction.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)220mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 5h at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). A mixed solution E of 1.0g of a 0.3% silica solution and 0.5g of an 8% PVA aqueous solution was mixed with a PVP aqueous solution of 2.0% by mass in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Fig. 6 is a surface 3D effect plot of an iridescent film prepared as described in this example. As can be seen from the figure, the amount of protrusions on the surface of the iridescent film is very small, and the surface of the iridescent film is extremely flat and uniform as compared with the iridescent film without PVP (see fig. 3), which indicates that the dispersion of silica is improved and the film formation is more uniform due to the PVP.
Example 10
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 60 ℃ and the reaction time was 10h, and a solution A was formed after the reaction.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)220mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 5h at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). A mixed solution E of 1.0g of a 0.3% silica solution and 0.5g of an 8% PVA aqueous solution was mixed with a 1.7% PVP aqueous solution in terms of mass ratio in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Fig. 7 is a surface 3D effect plot of an iridescent film prepared as described in this example. As can be seen from the figure, the surface flatness of the iridescent film was slightly reduced compared to the iridescent film with more PVP added (see fig. 6), but the film had improved silica dispersibility due to the addition of PVP compared to the iridescent film without PVP (see fig. 3), thereby greatly improving the film formation uniformity and flatness.
Example 11
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 60 ℃ and the reaction time was 10h, and a solution A was formed after the reaction.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)220mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 5h at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). A mixed solution E of 1.0g of a 0.3% silica solution and 0.5g of an 8% PVA aqueous solution was mixed with a 1.25% PVP aqueous solution in terms of mass ratio in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 12
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 60 ℃ and the reaction time was 10h, and a solution A was formed after the reaction.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)2O/no20mL of each of the mixed solution C of the aqueous ethanol and the ammonia water, the synthesis rate of the silicon dioxide is controlled bidirectionally, and the reaction is carried out for 5 hours at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). A mixed solution E of 1.0g of a 0.3% silica solution and 0.5g of an 8% PVA aqueous solution was mixed with a 1.0% PVP aqueous solution in terms of mass ratio in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 13
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 60 ℃ and the reaction time was 10h, and a solution A was formed after the reaction.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)220mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 5h at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). A mixed solution E of 1.0g of a 0.3% silica solution and 0.5g of an 8% PVA aqueous solution was mixed with a 0.7% PVP aqueous solution in terms of mass ratio in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 14
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 60 ℃ and the reaction time was 10h, and a solution A was formed after the reaction.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)220mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 5h at 25 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (5) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). A mixed solution E of 0.5g of a 0.3% silica solution and 1.5g of an 8% PVA aqueous solution was mixed with a 1.7% PVP aqueous solution in terms of mass ratio in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 15
(1) Adding 155mL of absolute ethyl alcohol, 30mL of deionized water and 8mL of ammonia water into a three-necked bottle; 8mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 65 ℃ and the reaction time was 10h, and a solution A was formed after the reaction was completed.
(2) Adding 155mL of absolute ethyl alcohol, 30mL of deionized water and 27mL of ammonia water into a three-necked bottle, stirring at a low rotating speed, adding 4.2 mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)223mL of O/absolute ethyl alcohol/ammonia water mixed solution C respectively, and bidirectional controlThe silica synthesis rate was made and the reaction was carried out at 35 ℃ for 4.5h to form solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 45 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). A mixed solution E of 0.5g of a 0.3% silica solution and 1.5g of an 8% PVA aqueous solution was mixed with a 0.7% PVP aqueous solution in terms of mass ratio in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 16
(1) 160mL of absolute ethyl alcohol, 26mL of deionized water and 5mL of ammonia water are added into a three-mouth bottle; 5mL of tetraethyl orthosilicate (TEOS) is slowly added, the reaction temperature is 60 ℃, the reaction time is 12 hours, and a solution A is formed after the reaction is finished.
(2) Adding 160mL of absolute ethyl alcohol, 32mL of deionized water and 32mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 8mL of the solution A obtained in the step (1), and continuously stirring to adjust the SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)2And (3) reacting the O/absolute ethyl alcohol/ammonia water mixed solution C with 17mL of each solution at 30 ℃ for 4 hours by controlling the synthesis rate of silicon dioxide bidirectionally to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 40 ℃ for 6 hours to obtain the silicon dioxide microspheres.
(5) And (4) preparing a suspension with the mass fraction of 0.4% by using the silicon dioxide obtained in the step (4). A mixed solution E of 0.5g of a 0.4% silica solution and 1.5g of an 8% PVA aqueous solution was mixed with a PVP aqueous solution of 2.0% by mass in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
Example 17
(1) Adding 150mL of absolute ethyl alcohol, 23mL of deionized water and 4mL of ammonia water into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 63 ℃ and the reaction time was 12h, and a solution A was formed after the reaction was completed.
(2) Adding 150mL of absolute ethyl alcohol, 26mL of deionized water and 26mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 4mL of the solution A obtained in the step (1), and continuously stirring to adjust SiO in the system2And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2)2And (3) respectively 21mL of O/absolute ethyl alcohol/ammonia water mixed solution C, bidirectionally controlling the synthesis rate of silicon dioxide, and reacting for 5 hours at 26 ℃ to form a solution D.
(4) And (4) centrifugally purifying the solution D obtained in the step (3) by adopting absolute ethyl alcohol, and drying at 45 ℃ for 7 hours to obtain the silicon dioxide microspheres.
(5) And (5) preparing a suspension with the mass fraction of 0.6% by using the silicon dioxide obtained in the step (4). A mixed solution E of 2g of a 0.6% silica solution and 1.5g of an 8% PVA aqueous solution was mixed with a 2.5% PVP aqueous solution in terms of mass ratio in the mixed solution to obtain a mixed solution F.
(6) Pouring the solution F obtained in the step (5) into a culture dish or dripping the solution F on a glass sheet, and drying at 40 ℃ to obtain the silica/PVA iridescent film.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. A method for preparing an optical film, comprising the steps of:
step 1, mixing absolute ethyl alcohol, water and ammonia water, and then dropwise adding tetraethoxysilane for reaction to generate a seed solution A;
step 2, mixing absolute ethyl alcohol, water and ammonia water, and adding the seed solution A to generate a reaction solution B;
step 3, adding tetraethoxysilane and the mixed solution C into the reaction solution B, and reacting to generate a solution D; the adding amount of the tetraethoxysilane and the mixed solution C is equal; the mixed solution C is a mixture of ammonia water, water and absolute ethyl alcohol;
step 4, purifying the solution D, drying and grinding the purified product to obtain silicon dioxide microspheres;
step 5, preparing a silicon dioxide suspension through silicon dioxide microspheres, and adding a PVA (polyvinyl acetate) aqueous solution and a PVP (polyvinyl pyrrolidone) aqueous solution into the silicon dioxide suspension to obtain a blending solution E;
and 6, obtaining the optical film with the silicon dioxide-based structural color by blending the solution E.
2. The method as claimed in claim 1, wherein in step 1, the volume ratio of the mixture of absolute ethanol, water and ammonia water is (150- & 160): (23-33): (4-8);
the reaction temperature is 60-65 ℃ and the reaction time is 10-12 h.
3. The method as claimed in claim 1, wherein in step 2, the mixing volume ratio of the absolute ethanol, the water and the ammonia water is (150- & 160): (26-32): (26-32).
4. The method of claim 1, wherein in the step 2, the mixing volume ratio of the seed solution A and the absolute ethyl alcohol is: (4-8): (150-160).
5. The method for preparing an optical film according to claim 1, wherein in step 3, the mixing ratio of the tetraethoxysilane to the seed solution in step 2 is (17-23): (4-8);
in the step 3, the volume ratio of the ammonia water to the absolute ethyl alcohol in the mixed solution C is 7:3: 10.
6. The method of claim 1, wherein in step 3, the reaction temperature is 25-35 ℃ and the reaction time is 4-5 h.
7. The method of claim 1, wherein in step 4, the drying temperature is 40-45 ℃ and the drying time is 6-10 h.
8. The method of claim 1, wherein in step 5, the silica microspheres are present in the silica suspension in an amount of 0.3% to 0.6% by weight.
9. The method of claim 1, wherein in step 5, the weight ratio of the PVP aqueous solution in the blending solution E is 0.7% -2.5%, and the weight ratio of the silica suspension to the PVA aqueous solution is (0.5-2.0): (0.5-1.5).
10. An optical film prepared by the preparation method of any one of claims 1 to 9, wherein the optical film is formed by pouring and self-assembling a blended solution, wherein the blended solution contains silica microspheres, and the particle size of the silica microspheres is 200-750 nm.
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