CN117924970A - Low-angle-dependence photonic crystal structural color material and preparation method thereof - Google Patents

Low-angle-dependence photonic crystal structural color material and preparation method thereof Download PDF

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Publication number
CN117924970A
CN117924970A CN202311679116.8A CN202311679116A CN117924970A CN 117924970 A CN117924970 A CN 117924970A CN 202311679116 A CN202311679116 A CN 202311679116A CN 117924970 A CN117924970 A CN 117924970A
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photonic crystal
crystal structure
color film
nano
suspension
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高伟洪
李月佳
陈凯凯
孙光武
潘斌杰
田红柳
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Shanghai University of Engineering Science
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D125/00Coating compositions based on 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 aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
    • C09D125/02Homopolymers or copolymers of hydrocarbons
    • C09D125/04Homopolymers or copolymers of styrene
    • C09D125/06Polystyrene
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0097Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B69/00Dyes not provided for by a single group of this subclass
    • C09B69/10Polymeric dyes; Reaction products of dyes with monomers or with macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • C09C1/30Silicic acid
    • C09C1/3009Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • C09C1/30Silicic acid
    • C09C1/3009Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
    • C09C1/3018Grinding
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3615Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3615Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C1/3623Grinding
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

The invention discloses a photonic crystal structure color material with low angle dependence and a preparation method thereof, comprising the following steps: adding the nano-microspheres into absolute ethyl alcohol, and performing ultrasonic dispersion to obtain nano-microsphere suspension; preparing the nano microsphere suspension into a photonic crystal structure color film by adopting a gravity sedimentation method; grinding the photonic crystal structure color film to obtain photonic crystal structure color film powder; dispersing photonic crystal structure color film powder in absolute ethyl alcohol to prepare photonic crystal suspension; carrying out ultrasonic treatment on the photonic crystal suspension; and (3) placing the suspension after ultrasonic treatment on the surface of a glass substrate, and performing self-assembly of dry colloid particles to obtain the photonic crystal structural color material with low angle dependence. The invention can obtain the photonic crystal structural color film with low angle dependence by using the nano particles with single particle diameter, and compared with the existing doping method and spraying method, the method is simpler, easy to operate and high-efficiency, and is beneficial to the application in dyeing.

Description

Low-angle-dependence photonic crystal structural color material and preparation method thereof
Technical Field
The invention relates to the field of photonic crystal structure color film materials, in particular to a photonic crystal structure color material with low angle dependence and a preparation method thereof.
Background
There are two main sources of color, chemical and structural. The chemical color is a color which is exhibited by that the chromophore, the color assisting group and other chemical groups absorb light with specific frequency, so that electrons are transited between molecular orbitals and photons with different frequencies are released, and the color is easy to fade with time or under illumination. Unlike chemical colors, the surface of an object with a structural color has a micro-nano structure with an optical scale, and can interact with light to generate optical effects such as reflection, refraction, scattering, diffraction, interference and the like, so that bright colors are generated. The characteristic of bright and non-fading structural color is the most widely focused of researchers.
The structural color is divided into photonic crystal structural color and amorphous photonic crystal structural color. However, due to the periodic arrangement structure of the photonic crystals, the generated color has the characteristic of angle dependence, which makes the application of the structural color material in the fields of textile, dye, imaging and the like limited to a certain extent. The amorphous photonic crystal structure is a special defect state structure of the photonic crystal, can generate structural color which is not influenced by an observation angle, and has wide potential application in the textile field.
The existing method for preparing the amorphous photonic crystal structural color mainly adopts a spraying method, a doping method, a core-shell structure method, a screen printing method and the like. Although many researches on methods for preparing amorphous photonic crystal structural colors are carried out at present, problems still exist, such as blockage of a spray gun when preparing structural colors by a spraying method; when the material is prepared by a doping method, at least two materials with different particle sizes are needed; the core-shell structure method is complex to construct and is not beneficial to mass preparation; when the amorphous photonic crystal is prepared by a screen printing method, the viscosity of the suspension is required to be high, and the industrial application of the amorphous photonic crystal structural color is limited.
Disclosure of Invention
An object of the present invention is to provide a method for preparing photonic crystal structural color material with low angle dependence.
It is another object of the present invention to provide photonic crystal structural color materials with low angle dependence prepared by the above method.
For this purpose, the invention adopts the following technical scheme:
a preparation method of a photonic crystal structural color material with low angle dependence comprises the following steps:
s1, adding the nano-microspheres into absolute ethyl alcohol, and performing ultrasonic dispersion to obtain nano-microsphere suspension with the concentration of 20-30 mg/ml;
s2, preparing the nano microsphere suspension obtained in the step S1 into a photonic crystal structure color film by adopting a gravity sedimentation method;
s3, grinding the photonic crystal structure color film obtained in the step S2 to obtain photonic crystal structure color film powder, wherein the particle size of the photonic crystal structure color film powder is 407-523 nm;
s4, dispersing the photonic crystal structural color film powder obtained in the S3 in absolute ethyl alcohol to prepare a photonic crystal suspension with the concentration of 20-30 mg/ml;
S5, carrying out ultrasonic treatment on the photonic crystal suspension obtained in the step S4;
s6, the suspension after the ultrasonic treatment of S5 is taken and placed on the surface of the glass substrate, and the glass substrate is placed in a temperature-stable oven for self-assembly of dry colloid particles, so that the photonic crystal structural color material with low angle dependence is prepared.
In S1, the nano microsphere is SiO 2, PS or TiO 2 nano microsphere, the particle size of the nano microsphere is uniform, and the particle size is 198-314nm.
In S1, the particle size dispersion coefficient (PDI) of the nano-microsphere is less than 0.1.
In S1, the ultrasonic dispersion time is 50-90min.
In S3, the grinding time is 30-40min.
In S5, the ultrasonic time is 50-60min.
In S6, the temperature of the oven is 40-60 ℃.
In S6, the volume of the suspension was 4ml.
The invention prepares the photonic crystal structural color material with low angle dependence by redispersing the nano-sphere structural color film with the particle size. According to the invention, the photonic crystal structure color film is prepared by a gravity sedimentation method, and finally the photonic crystal structure color film is ground, dispersed, ultrasonically treated and self-assembled by dry colloid particles by a redispersion method, so that the photonic crystal structure color material with low angle dependence is prepared.
Compared with the prior art, the invention has the following beneficial effects:
1. The invention can obtain the photonic crystal structural color film with low angle dependence by using the nano particles with single particle diameter, and compared with the existing doping method and spraying method, the method is simpler, easy to operate and high-efficiency, and is beneficial to the application in dyeing.
2. The method is not only suitable for SiO 2, but also suitable for other nano-microspheres, such as uniform microspheres of titanium dioxide (TiO 2), polystyrene (PS) and the like, so that the method is expected to realize the industrial production of photonic crystal structural color.
Drawings
FIG. 1 is a graph showing the low angle dependence of the photonic crystal structure color film prepared in example 1 and the photonic crystal structure color film prepared in comparative example 1 under different observation angles, wherein (a) in FIG. 1 is the photonic crystal structure color film with low angle dependence, and (b) in FIG. 1 is the photonic crystal structure color film prepared in comparative example 1;
FIG. 2 is a reflectance spectrum of the photonic crystal structural color film with low angle dependence prepared in example 1;
FIG. 3 is a reflectance spectrum of the photonic crystal structural color film prepared in comparative example 1;
FIG. 4 is a photonic crystal structure color textile with low angle dependence prepared in example 4;
Fig. 5 (a) and (b) are respectively SEM images and 2D-FFT conversion images of the photonic crystal structure color thin film prepared in comparative example 1, and fig. 5 (c) and (D) are respectively SEM images and 2D-FFT conversion images of the photonic crystal structure color thin film prepared in example 1 with low angle dependence.
Detailed Description
The technical scheme of the invention is described in detail below with reference to the accompanying drawings and examples.
Example 1
A preparation method of a photonic crystal structure color film with low angle dependence comprises the following steps:
S1, adding SiO 2 nano-microspheres (PDI is 0.013) with the particle size of 314nm into absolute ethyl alcohol, and performing ultrasonic dispersion for 60min to prepare SiO 2 nano-microsphere suspension with the concentration of 25 mg/ml;
S2, preparing a photonic crystal structure color film from the SiO 2 nano microsphere suspension obtained in the step S1 by a gravity sedimentation method;
S3, grinding the photonic crystal structure color film obtained in the step S2 for 30min to obtain photonic crystal structure color film powder (the particle size is 523 nm);
s4, dispersing the photonic crystal structure color film powder obtained in the step S3 in absolute ethyl alcohol to obtain a photonic crystal suspension with the concentration of 25 mg/ml;
s5, carrying out ultrasonic treatment on the photonic crystal suspension in the step S4 for 50min;
and S6, placing 4ml of the suspension liquid subjected to ultrasonic treatment in the step S5 on the surface of a glass substrate, and placing the glass substrate in a baking oven at 40 ℃ for self-assembly of dry colloid particles to prepare the SiO 2 amorphous photonic crystal structure color film.
Comparative example 1
The preparation method of the photonic crystal structure color film comprises the following steps:
S1, adding SiO 2 nano-microspheres with the particle size of 314nm into absolute ethyl alcohol, and performing ultrasonic dispersion for 60min to prepare SiO 2 nano-microsphere suspension with the concentration of 25 mg/ml;
S2, preparing the SiO 2 nanometer microsphere suspension obtained in the step S1 into a photonic crystal structure color film by a gravity sedimentation method.
Example 2
A preparation method of a photonic crystal structure color film with low angle dependence comprises the following steps:
s1, adding PS nano-microspheres (PDI is less than 0.1) with the particle size of 265nm into absolute ethyl alcohol, and performing ultrasonic dispersion for 60min to prepare PS nano-microsphere suspension with the concentration of 25 mg/ml;
s2, preparing a photonic crystal structure color film from the PS nano microsphere suspension obtained in the step S1 by a gravity sedimentation method;
S3, grinding the photonic crystal structure color film obtained in the step S2 for 30min to obtain photonic crystal structure color film powder (the particle size is 493 nm);
s4, dispersing the photonic crystal structure color film powder obtained in the step S3 in absolute ethyl alcohol to obtain a photonic crystal suspension with the concentration of 25 mg/ml;
S5, carrying out ultrasonic treatment on the photonic crystal suspension in the step S4 for 50min;
S6, taking 4ml of the suspension obtained in the step S5, placing the suspension on the surface of a glass substrate, and placing the glass substrate in a baking oven at 40 ℃ for self-assembly of dry colloid particles to prepare the PS amorphous photonic crystal structural color film.
Example 3
A preparation method of a photonic crystal structure color film with low angle dependence comprises the following steps:
S1, adding TiO 2 nano-microspheres (PDI is less than 0.1) with the particle size of 198nm and uniform size into absolute ethyl alcohol, and performing ultrasonic dispersion for 60min to prepare TiO 2 nano-microsphere suspension with the concentration of 25 mg/ml;
S2, preparing a photonic crystal structure color film from the TiO 2 nano microsphere suspension obtained in the step S1 by a gravity sedimentation method;
S3, grinding the photonic crystal structure color film obtained in the step S2 for 30min to obtain photonic crystal structure color film powder (the particle size is 407 nm);
s4, dispersing the photonic crystal structure color film powder obtained in the step S3 in absolute ethyl alcohol to obtain a photonic crystal suspension with the concentration of 25 mg/ml;
S5, carrying out ultrasonic treatment on the photonic crystal suspension in the step S4 for 50min;
S6, placing 4ml of the suspension liquid subjected to ultrasonic treatment in the step S5 on the surface of a glass substrate, and placing the glass substrate in a baking oven at 40 ℃ for self-assembly of dry colloid particles to prepare the TiO 2 amorphous photonic crystal structure color film.
Example 4
A preparation method of photonic crystal structure color fabric with low angle dependence comprises the following steps:
S1, adding SiO 2 nano-microspheres (PDI is 0.029) with the particle size of 256nm into absolute ethyl alcohol, and performing ultrasonic dispersion for 60min to prepare SiO 2 nano-microsphere suspension with the concentration of 25 mg/ml;
S2, preparing a photonic crystal structure color film from the SiO 2 nano microsphere suspension obtained in the step S1 by a gravity sedimentation method;
s3, grinding the photonic crystal structure color film obtained in the step S2 for 30min to obtain photonic crystal structure color film powder (the particle size is 452 nm);
s4, dispersing the photonic crystal structure color film powder obtained in the step S3 in absolute ethyl alcohol to obtain a photonic crystal suspension with the concentration of 25 mg/ml;
s5, carrying out ultrasonic treatment on the photonic crystal suspension in the step S4 for 50min;
S6, placing 4ml of the suspension liquid subjected to ultrasonic treatment in the step S5 on the surface of the black polyester plain weave fabric, and placing the black polyester plain weave fabric into a baking oven at 40 ℃ for self-assembly of dry colloid particles to prepare the SiO 2 amorphous photonic crystal structure colored fabric.
Fig. 1 (a) is a photograph of a photonic structure color film with low angle dependence prepared by a redispersion method, and fig. 1 (b) is a photograph of a photonic crystal structure color film. It can be found that the color of the photonic crystal structure color film changes from red to yellow with increasing viewing angle from 0 ° vertical angle to 60 ° viewing angle; the low angle-dependent photonic structure color film prepared by the redispersion method has a low color change from a vertical angle of 0 ° to an observation angle of 60 °. As can be seen from the reflectivity wave diagrams shown in fig. 2 and 3, the reflectivity wave peak of the reflectivity wave diagram of the photonic crystal structure color film is blue shifted from the vertical angle of 0 ° to the observation angle of 60 °; the reflectance peaks of the reflectance spectrum of the photonic structure color film with low angle dependence prepared by the redispersion method are almost unchanged, so that the structural color film with low angle dependence of photons prepared by the redispersion method is proved to have better low angle dependence.
As shown in fig. 5 (a) and (b), it can be seen that SiO 2 nanoparticles are spherical and have a uniform particle size distribution, and SiO 2 nanoparticles are orderly arranged between them. SEM and fourier transform (2D-FFT) analysis of the red SiO 2 photonic crystal structure color film using Image J software revealed that the 2D-FFT pattern in fig. 5 (b) all exhibited a hexagonal symmetric crystal structure with anisotropy. As shown in fig. 5 (c) and (D), unlike the ordered arrangement of photonic crystal structures in fig. 5 (a) and (b), the non-photonic crystal exhibits a long-range disordered crystal structure, and such an amorphous crystal structure results in low angle dependence, and the central symmetrical circle in the 2D-FFT plot of fig. 5 (D) also characterizes such an isotropic amorphous structure. Again, the feasibility of redispersion methods to produce photonic crystal structure color materials with low angular dependence was demonstrated.

Claims (8)

1. A method for preparing a photonic crystal structural color material with low angle dependence, which is characterized by comprising the following steps:
S1, adding nano-microspheres into absolute ethyl alcohol, and performing ultrasonic dispersion to prepare nano-microsphere suspension with the concentration of 20-30 mg/ml;
S2, preparing the nano microsphere suspension obtained in the step S1 into a photonic crystal structure color film by adopting a gravity sedimentation method;
s3, grinding the photonic crystal structure color film obtained in the step S2 to obtain photonic crystal structure color film powder, wherein the particle size of the photonic crystal structure color film powder is 407-523 nm;
s4, dispersing the photonic crystal structure color film powder obtained in the step S3 in absolute ethyl alcohol to prepare a photonic crystal suspension with the concentration of 20-30 mg/ml;
S5, carrying out ultrasonic treatment on the photonic crystal suspension obtained in the step S4;
S6, the suspension liquid after ultrasonic treatment in the step S5 is taken and placed on the surface of a glass substrate, and the glass substrate is placed in a temperature-stable oven for self-assembly of dry colloid particles, so that the photonic crystal structural color material with low angle dependence is prepared.
2. The method according to claim 1, wherein in the step S1, the nano-microsphere is SiO 2, PS or TiO 2 nano-microsphere, the nano-microsphere has a uniform particle size, and the particle size is 198-314nm.
3. The method according to claim 1, wherein in step S1, the nanoparticle has a particle size dispersion coefficient (PDI) of < 0.1.
4. The method according to claim 1, wherein in step S1, the ultrasonic dispersion is performed for 50 to 90 minutes.
5. The method according to claim 1, wherein the grinding time is 30-40min in step S3.
6. The method according to claim 1, wherein in step S5, the ultrasonic time is 50-60min.
7. The method according to claim 1, wherein in step S6, the temperature of the oven is 40-60 ℃.
8. The method of claim 1, wherein in step S6, the suspension has a volume of 4ml.
CN202311679116.8A 2023-12-07 2023-12-07 Low-angle-dependence photonic crystal structural color material and preparation method thereof Pending CN117924970A (en)

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