CN105111480A - Orange-yellow photonic crystal structural color film with photocatalytic effect and preparation method of film - Google Patents
Orange-yellow photonic crystal structural color film with photocatalytic effect and preparation method of film Download PDFInfo
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- CN105111480A CN105111480A CN201510604282.0A CN201510604282A CN105111480A CN 105111480 A CN105111480 A CN 105111480A CN 201510604282 A CN201510604282 A CN 201510604282A CN 105111480 A CN105111480 A CN 105111480A
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Abstract
The invention discloses an orange-yellow photonic crystal structural color film with a photocatalytic effect and a preparation method of the film, and belongs to the technical field of preparation of photonic crystal structural color films. According to the preparation method, zinc sulphide microspheres with a uniform particle diameter are prepared according to a uniform deposition method at first, and then the orange-yellow photonic crystal structural color film is self-assembled on the surface of a glass matrix according to a vertical deposition method. The orange-yellow photonic crystal structural color film is bright in color and low in color fading possibility, overcomes the defects that chemical organic pigments are high in color fading possibility and harmful to human health, and achieves the function of conducting photocatalytic degradation on Rhodamine B. The orange-yellow photonic crystal structural color film and the preparation method have the advantages that the technological process is simple and feasible, large-scale industrial production can be achieved, and the application prospect is broad.
Description
Technical field
The invention belongs to photonic crystal structure color film preparing technical field, be specifically related to a kind of preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect.
Background technology
Photonic crystal is that dielectric refractive index periodical change causes photonic band gap structure, thus controls light motion in the photonic crystal by photonic band gap structure.Photonic crystal is the material of the appearance low-refraction of some positional cycle in high-index material.The materials arranged in alternating of high low-refraction forms periodic structure and just can produce photonic band gap.Thus create schemochrome.This is a kind of physics colour generation, and it has the advantages such as bright-colored, will never fade, environmental friendliness, preparation cycle are short.Wherein by the orderly self-assembly method of colloid micro ball, just photonic crystal of opals structure can be formed, there is photon band gap feature, when incident light frequency drops in bandgap range, this incident light will by this photonic crystal, these visible rays that can not continue to propagate can be reflected by photonic crystal, finally form coherent diffraction at the photon crystal surface with periodic structure, and produce bright and colourful schemochrome.By the research to occurring in nature and artificial preparation schemochrome, there is good application in display, decoration, the field such as false proof at present.As Chinese invention patent application CN201310205537.7 discloses a kind of preparation method of red photon crystalline structure color glaze, mainly obtained on ceramic body surface by the self-assembling technique of silicon dioxide microsphere, this red photon crystalline structure look has good colouring effect.Disclose a kind of hydrothermal method in Chinese invention patent application CN201010276061.2 and prepare zinc sulphide microballoon, and announce this zinc sulphide microballoon there is good ultraviolet light response.
But, be only limitted to the imitated of different colours colouring effect to the research of photonic crystal structure color film at present and analyze, main material is then silicon oxide, the materials such as polystyrene, to polyfunctional photonic crystal structure color material, particularly very few to the photonic crystal structure color film research with photocatalysis performance.
Summary of the invention
The object of the present invention is to provide a kind of bright-colored, will never fade, and orange-yellow photonic crystal structure color film with photocatalytic effect and preparation method thereof.
The present invention is achieved through the following technical solutions:
The invention discloses a kind of preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect, comprise the following steps:
1) by 15:(1 ~ 2) mass ratio, take Zn (NO
3)
26H
2o and polyvinylpyrrolidone, after mixing, by Zn (NO
3)
26H
2o: the ratio of deionized water=(0.3 ~ 0.5) g:100mL adds deionized water, stirs, obtains homogeneous solution;
2) by the amount ratio of (0.2 ~ 0.4) g:50mL, thioacetamide is added in deionized water, ultrasonicly to mix, obtain thioacetyl amine aqueous solution;
3) by step 1) and 2) obtained two solution, by (1 ~ 2): after the volume ratio mixing of 1, at 80 ~ 95 DEG C, stirring in water bath reaction 5 ~ 7h, obtain the emulsion containing zinc sulphide microballoon, again through washing, alcohol wash and ultrasonic disperse process, obtain the alcoholic solution of monodisperse ZnS microballoon;
4) slide glass of cleaning is vertically positioned over step 3) in the alcoholic solution of obtained monodisperse ZnS microballoon; at 40 ~ 60 DEG C; after vacuum drying treatment to alcohol volatilization completely; orange-yellow photonic crystal structure color film is generated in slide surface; again under nitrogen protection through 300 ~ 500 DEG C of thermal treatments, the obtained orange-yellow photonic crystal structure color film with photocatalytic effect.
Step 1) stir employing magnetic stirrer process 20 ~ 35min.
Step 2) in ultrasonic mixing time be 10 ~ 20min.
Step 3) in washing, alcohol wash be the emulsion containing zinc sulphide microballoon is used successively water and ethanol purge three times.
Step 3) in the ultrasonic disperse time be 10 ~ 20min.
Step 4) described in the slide glass of cleaning be that slide glass is placed in H
2sO
4with H
2o
2in the aqueous solution by volume for 7:3 preparation, soak 30min, then clean with distilled water, dry obtained at 60 DEG C.
Step 4) in the vacuum drying treatment time be 35 ~ 45h.
Step 4) in heat treatment time be 1 ~ 3h.
The invention also discloses the orange-yellow photonic crystal structure color film with photocatalytic effect adopting above-mentioned method to obtain.
Compared with prior art, the present invention has following useful technique effect:
The preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect disclosed by the invention, first adopts sluggish precipitation, by strict control Zn (NO
3)
26H
2the reaction ratio (mass ratioes of 15:1 ~ 2) of O and polyvinylpyrrolidone, and the consumption of the deionized water added, prepare the emulsion containing zinc sulphide microballoon, zinc sulphide microspherulite diameter is 280 ± 10nm; Then vertical deposition method is adopted to become orange-yellow photonic crystal structure color film at glass basis surface self-organization.This schemochrome orange-yellow film color is beautiful, not fugitive color, solves chemical organic compounds pigment fugitive color, harmful shortcoming.And achieve the photocatalytic degradation function of photonic crystal structure color film to rhodamine B.Present invention process process is simple, and energy large-scale commercial production, has broad application prospects.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram that embodiment 1 gained has the orange-yellow schemochrome film of photocatalytic effect;
Fig. 2 is the reflected light spectrogram that embodiment 1 gained has the orange-yellow schemochrome film of photocatalytic effect;
Fig. 3 is the rhodamine B photocatalytic degradation figure that embodiment 1 gained has the orange-yellow photonic crystal structure color film of photocatalytic effect.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Embodiment 1
There is a preparation method for the orange-yellow photonic crystal structure color film of photocatalytic effect, comprise the following steps:
(1) in mass ratio for 15:1 takes Zn (NO
3)
26H
2o and polyvinylpyrrolidone (PVP) some grams, add in beaker, proportionally 0.45gZn (NO
3)
26H
2o:100mL deionized water, magnetic agitation is fully dissolved and Homogeneous phase mixing, stirs 30min and just obtains homogeneous solution.
(2) precise thioacetamide 0.3g, adds the ultrasonic mixing 10 ~ 20min of 50mL deionized water, obtains thioacetyl amine aqueous solution.
(3) after above-mentioned (1) and (2) two solution being stirred respectively, add in same beaker, and at 90 DEG C of Water Under bath reaction 6h on magnetic agitation instrument, can obtain obtaining emulsion containing zinc sulphide microballoon.Obtain the ethanolic soln of monodisperse ZnS microballoon through ultrasonic disperse after washing, alcohol wash each three are taken second place.
(4) slide glass of a certain size (25.6 × 76.2mm) is placed in H
2sO
4/ H
2o
2(7:3V/V) soak 30min in the aqueous solution, then take out and clean with a large amount of distilled water, finally dry in 60 DEG C of baking ovens, save backup.
Cleaned slide glass is vertically positioned in the ZnS microballoon emulsion obtained by step 3, and whole system is placed in constant temperature (40 ~ 60 DEG C ± 1 DEG C) vacuum drying oven, approximately pass through 40h, after ethanol volatilization completely, a kind of orange-yellow photonic crystal structure color film with photocatalytic effect will be generated at glass substrate surface.Under nitrogen protection through 500 DEG C of thermal treatments, the zinc sulphide photon crystal film with photocatalysis performance can be obtained.
As follows to the testing method of the orange-yellow photonic crystal structure color film color generation property that the present embodiment obtains:
The reflection spectrum of ultraviolet-visible-near-infrared spectrum instrument is adopted to analyze, INSTRUMENT MODEL: Lamda950 type, Beckman company of the U.S., wavelength region 175 ~ 3300nm, bandwidth 0.5 ~ 5.0nm, stray light <0.00008%T, wavelength accuracy 0.08nm, scan three times, average.
In the present invention, the testing method of orange-yellow photonic crystal structure color film photocatalysis performance is as follows:
Photocatalytic degradation rhodamine B solution, rhodamine B solution 40 ~ 80ml and step 4 that concentration is 10mg/L is added in light-catalyzed reaction instrument) film size that obtains is the orange-yellow photonic crystal structure color film with photocatalytic effect of 1cm × 2cm, 10min is reacted subsequently in unglazed darkroom, ZnS microballoon and rhodamine B reaction solution are fully mixed, reaches absorption/desorption equilibrium.Open the mercury lamp of 500W after light-catalyzed reaction starts, and at the uniform velocity stirred by magnetic stirring apparatus, every 10min sampling, measure organic degradation effect by the absorbancy of reaction solution.Absorbancy adopts Lambda-950 type ultraviolet-visible spectrometer to measure.
Using the ratio of rhodamine B solution starting point concentration in the concentration and its solution of t as the degradation rate of the solution that is degraded, characterize the Photocatalytic Degradation Property of ZnS microballoon respectively:
C/C
0＝A/A
0
In formula, C
0represent that reaction starts the concentration of solution when the concentration of front solution and photochemical catalysis start rear reaction t time respectively with C, A
0the absorbance at the absorbing wavelength place that solution is maximum when representing that reaction starts front and light-catalyzed reaction t time respectively with A.
Its XRD analysis of sample of the orange-yellow zinc sulphide photonic crystal structure color film obtained through the present embodiment as shown in Figure 1, its XRD analysis as shown in Figure 1,2 θ=28.2 °, 47.7 °, (111) of 56.6 ° of corresponding ZnS of difference, (220), (311) crystal face, and except ZnS characteristic peak, do not have other assorted peaks to occur, show that prepared sample is pure ZnS.; As shown in Figure 2, as can be seen from the figure, the reflection peak of zinc sulphide schemochrome film is in orange-yellow scope for reflection spectrum.As shown in Figure 3, as can be seen from the figure prepared zinc sulphide has good degradation effect to organic dye rhodamine B in photocatalytic effect analysis, substantially can by rhodamine B degraded completely in 60min.
Embodiment 2
There is a preparation method for the orange-yellow photonic crystal structure color film of photocatalytic effect, comprise the following steps:
(2) in mass ratio for 15:2 takes Zn (NO
3)
26H
2o and polyvinylpyrrolidone (PVP) some grams, add in beaker, proportionally 0.5gZn (NO
3)
26H
2the ratio of O:100mL deionized water adds deionized water, and magnetic agitation is fully dissolved and Homogeneous phase mixing, stirs 30min and just obtains homogeneous solution.
(2) precise thioacetamide 0.3g, adds the ultrasonic mixing 10 ~ 20min of 50mL deionized water, obtains thioacetyl amine aqueous solution.
(3) after above-mentioned (1) and (2) two solution being stirred respectively, add in same beaker, and at 80 DEG C of Water Under bath reaction 7h on magnetic agitation instrument, can obtain obtaining emulsion containing zinc sulphide microballoon.Obtain the ethanolic soln of monodisperse ZnS microballoon through ultrasonic disperse after washing, alcohol wash each three are taken second place.
(4) slide glass of a certain size (25.6 × 76.2mm) is placed in H
2sO
4/ H
2o
2(7:3V/V) soak 30min in the aqueous solution, then take out and clean with a large amount of distilled water, finally dry in 60 DEG C of baking ovens, save backup.
Cleaned slide glass is vertically positioned in the ZnS microballoon emulsion obtained by step 3, and whole system is placed in constant temperature (40 ~ 60 DEG C ± 1 DEG C) vacuum drying oven, approximately pass through 40h, after ethanol volatilization completely, a kind of orange-yellow photonic crystal structure color film with photocatalytic effect will be generated at glass substrate surface.Under nitrogen protection through 500 DEG C of thermal treatments, the zinc sulphide photon crystal film with photocatalysis performance can be obtained.
Embodiment 3
There is a preparation method for the orange-yellow photonic crystal structure color film of photocatalytic effect, comprise the following steps:
(3) in mass ratio for 15:1.5 takes Zn (NO
3)
26H
2o and polyvinylpyrrolidone (PVP) some grams, add in beaker, proportionally 0.5gZn (NO
3)
26H
2the ratio of O:100mL adds deionized water, and magnetic agitation is fully dissolved and Homogeneous phase mixing, stirs 30min and just obtains homogeneous solution.
(2) precise thioacetamide 0.2g, adds the ultrasonic mixing 10 ~ 20min of 50mL deionized water, obtains thioacetyl amine aqueous solution.
(3) after above-mentioned (1) and (2) two solution being stirred respectively, add in same beaker, and at 95 DEG C of Water Under bath reaction 5h on magnetic agitation instrument, can obtain obtaining emulsion containing zinc sulphide microballoon.Obtain the ethanolic soln of monodisperse ZnS microballoon through ultrasonic disperse after washing, alcohol wash each three are taken second place.
(4) slide glass of a certain size (25.6 × 76.2mm) is placed in H
2sO
4/ H
2o
2(7:3V/V) soak 30min in the aqueous solution, then take out and clean with a large amount of distilled water, finally dry in 40 DEG C of baking ovens, save backup.
Cleaned slide glass is vertically positioned in the ZnS microballoon emulsion obtained by step 3, and whole system is placed in constant temperature (40 ~ 60 DEG C ± 1 DEG C) vacuum drying oven, approximately pass through 40h, after ethanol volatilization completely, a kind of orange-yellow photonic crystal structure color film with photocatalytic effect will be generated at glass substrate surface.Under nitrogen protection through 300 DEG C of thermal treatments, the zinc sulphide photon crystal film with photocatalysis performance can be obtained.
Claims (9)
1. there is a preparation method for the orange-yellow photonic crystal structure color film of photocatalytic effect, it is characterized in that, comprise the following steps:
1) by 15:(1 ~ 2) mass ratio, take Zn (NO
3)
26H
2o and polyvinylpyrrolidone, after mixing, by Zn (NO
3)
26H
2o: the ratio of deionized water=(0.3 ~ 0.5) g:100mL adds deionized water, stirs, obtains homogeneous solution;
2) by the amount ratio of (0.2 ~ 0.4) g:50mL, thioacetamide is added in deionized water, ultrasonicly to mix, obtain thioacetyl amine aqueous solution;
3) by step 1) and 2) obtained two solution, by (1 ~ 2): after the volume ratio mixing of 1, at 80 ~ 95 DEG C, stirring in water bath reaction 5 ~ 7h, obtain the emulsion containing zinc sulphide microballoon, again through washing, alcohol wash and ultrasonic disperse process, obtain the alcoholic solution of monodisperse ZnS microballoon;
4) slide glass of cleaning is vertically positioned over step 3) in the alcoholic solution of obtained monodisperse ZnS microballoon; at 40 ~ 60 DEG C; after vacuum drying treatment to alcohol volatilization completely; orange-yellow photonic crystal structure color film is generated in slide surface; again under nitrogen protection through 300 ~ 500 DEG C of thermal treatments, the obtained orange-yellow photonic crystal structure color film with photocatalytic effect.
2. the preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect according to claim 1, is characterized in that, step 1) stir employing magnetic stirrer process 20 ~ 35min.
3. the preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect according to claim 1, is characterized in that, step 2) in ultrasonic mixing time be 10 ~ 20min.
4. the preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect according to claim 1, is characterized in that, step 3) in washing, alcohol wash be the emulsion containing zinc sulphide microballoon is used successively water and ethanol purge three times.
5. the preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect according to claim 1, is characterized in that, step 3) in the ultrasonic disperse time be 10 ~ 20min.
6. the preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect according to claim 1, is characterized in that, step 4) described in the slide glass of cleaning be that slide glass is placed in H
2sO
4with H
2o
2in the aqueous solution by volume for 7:3 preparation, soak 30min, then clean with distilled water, dry obtained at 60 DEG C.
7. the preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect according to claim 1, is characterized in that, step 4) in the vacuum drying treatment time be 35 ~ 45h.
8. the preparation method with the orange-yellow photonic crystal structure color film of photocatalytic effect according to claim 1, is characterized in that, step 4) in heat treatment time be 1 ~ 3h.
9. adopt the orange-yellow photonic crystal structure color film with photocatalytic effect that the method in claim 1 ~ 8 described in any one obtains.
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2015
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| US20040146811A1 (en) * | 2003-01-23 | 2004-07-29 | Seung-Man Yang | Method of preparing patterned colloidal crystals |
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