CN105271796A - Low angle dependence blue ZnS structural color film and preparation method thereof - Google Patents
Low angle dependence blue ZnS structural color film and preparation method thereof Download PDFInfo
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- CN105271796A CN105271796A CN201510604283.5A CN201510604283A CN105271796A CN 105271796 A CN105271796 A CN 105271796A CN 201510604283 A CN201510604283 A CN 201510604283A CN 105271796 A CN105271796 A CN 105271796A
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Abstract
The present invention discloses a low angle dependence blue ZnS structural color film and a preparation method thereof, and belongs to the technical field of the preparation of the structural color material. The method is as follows: first, chemical homogeneous precipitation method is used to prepare uniform size ZnS microsphere nanoparticles, a film is produced on glass or ceramic substrate surface, and the film is calcined in a reducing atmosphere for protection, so that trace organics are carbonized to obtain the blue structural color film with uniform distributed carbon black. The method is simple, and highly repetitive, solves the technical problems that organic chemical paint is easy to fade and harmful to human body, meanwhile overcomes problems of high substrate requirements, harsh coating conditions and the like of opal structure photonic crystal, is suitable for construction of angle-dependent color-variable structural color pigments on surface of a variety of materials, and has broad application prospects. The prepared blue ZnS structural color film has uniform distributed carbon black, no angle dependence, good sphericity, and uniform particle size.
Description
Technical field
The invention belongs to photon crystal material preparing technical field, be specifically related to a kind of low angle dependency blue zinc sulphide schemochrome film and preparation method thereof.
Background technology
The materials arranged in alternating of high low-refraction forms periodic structure, i.e. photonic crystal, and the light of specific wavelength does not produce photon band gap by it, thus creates schemochrome.Schemochrome is a kind of physics colour generation, has the advantages such as bright-colored, will never fade, environmental friendliness, preparation cycle are short.In the last few years by the orderly self-assembly method of colloid micro ball, photonic crystal of opals structure can be formed, the effects such as last light is formed by dryly to penetrate at the photon crystal surface with periodic structure, diffraction, scattering, thus produce bright and colourful schemochrome, but because have rainbow effect, namely the color observed of different directions is different, thus greatly limit schemochrome in flat pannel display, the application of the wide viewing angle such as printed medium and optical device display aspect.There is investigator to propose to add micro-black pigment and can improve colorimetric purity, and effectively can reduce the dependency of schemochrome to angle, reach the effect (CN103173039A along with viewing angle change schemochrome remains unchanged, 102702791A, 103788770A), but the weak point of aforesaid method is, in photonic crystal structure color film preparation, powder is needed to mix masking with micro-carbon black or black pigment, technique is more complicated, and opal structural requires very high to film coating environment, large by external environmental interference, very little environmental fluctuating all can have a great impact the quality of film, therefore be difficult to be widely used.Many researchers adds carbon black or the melanochrome of trace in silicon oxide or polystyrene colloidal liquid solution, the methods such as spin coating are utilized to prepare short range order, the schemochrome film of longrange disorder, wherein carbon black or melanic effect are can there be stronger absorption in visible light wave range, thus reduction non-coherent scattering, make schemochrome film in short range order, also higher colorimetric purity can be shown under the state of longrange disorder, this short range order simultaneously, the structure of longrange disorder is because isotropy, so have low angle dependency, namely along with the change of viewing angle, color is substantially constant, display can be applied to, the aspects such as printing.But, the ultrafine nanometer carbon black applied in this process has higher surface energy, therefore there is difficult dispersion, easily reunite, and in most solution, be difficult to the shortcomings such as dissolving, and organic black dyes needs to carry out the technological process such as colorant match, colour mixture, the shortcomings such as the complicated and organic black dyes prepared of process is unstable.In the last few years, semiconductor sulfide (such as zinc sulphide) material had a lot of excellent Performance Ratios as in sewage disposal because of it, and magneto-optic is changed, and antibacterial, the aspects such as photonic crystal are subject to extensive concern.
So far, document is not also had to carry out report to materials such as utilizing inorganic semiconductor oxide compound, sulfide to prepare this shot-range ordered structure look film.
Summary of the invention
In order to overcome the defect that above-mentioned prior art exists, the object of the present invention is to provide a kind of low angle dependency blue zinc sulphide schemochrome film and preparation method thereof, the method is simple to operate, and repeatability is strong, is applicable to commercial scale production; Through the obtained spherical degree of spherical zine sulfide photonic crystal of the method well, uniform particle diameter, is widely used.
The present invention is achieved through the following technical solutions:
The invention discloses the preparation method of the blue zinc sulphide photonic crystal structure color film of a kind of low angle dependency, comprise the following steps:
1) by (3 ~ 5): the mass ratio of 1 gets Zn (NO
3)
26H
2o and polyvinylpyrrolidone, then in polyvinylpyrrolidone: the ratio of deionized water=(0.05 ~ 0.06) g:100mL adds deionized water, fully mixes, obtains homogeneous solution;
2) in the ratio of (0.3 ~ 0.5) g:50mL, thioacetamide is dissolved in deionized water, ultrasonic combination treatment, obtains thioacetyl amine aqueous solution;
3) by step 1) obtained homogeneous solution and step 2) obtained thioacetyl amine aqueous solution presses (2 ~ 2.5): after the volume ratio of 1 mixes, at 70 ~ 85 DEG C, water-bath 5 ~ 8h, the obtained emulsion containing zinc sulphide microballoon, again through washing and ultrasonic disperse, the ethanolic soln of obtained monodisperse ZnS microballoon;
4) substrate is placed in the vacuum-drying of monodisperse ZnS microballoon ethanolic soln, obtained zinc sulfide film, by zinc sulfide film under protective atmosphere, through 300 ~ 500 DEG C of calcination processing, obtained blue zinc sulphide photonic crystal structure color colorant.
Step 1) fully to mix be adopt magnetic stirrer 25 ~ 30min.
Step 2) in the ultrasonic combination treatment time be 10 ~ 20min.
Step 3) described in washing be by the emulsion containing zinc sulphide microballoon first through deionization washing 2 ~ 4 times, then through washes of absolute alcohol 2 ~ 4 times.
Step 4) described protective atmosphere adopts nitrogen or argon gas.
Step 4) described vacuum-drying carries out at 50 ~ 65 DEG C.
The invention also discloses the blue zinc sulphide photonic crystal structure color film of the low angle dependency adopting aforesaid method obtained, this low angle dependency blue zinc sulphide photonic crystal structure color film carbon black is evenly distributed, non-angular dependency, good sphericity, uniform particle diameter.
Compared with prior art, the present invention has following useful technique effect:
The preparation method of low angle dependency disclosed by the invention blue zinc sulphide schemochrome film, first adopts the chemical homogeneous precipitator method, by strict control Zn (NO
3)
26H
2the reaction ratio (3 ~ 5:1) of O and polyvinylpyrrolidone; and the consumption of deionized water; prepare the zinc sulphide microsphere nano particle of uniform particle diameter; then calcination processing under protective atmosphere; micro-content organism is carbonized, thus obtains carbon black and be evenly distributed on blue schemochrome film in microballoon, the color of this carbon containing zinc sulphide microballoon film pigment can not change with the change of viewing angle; in colour-stable, not fugitive color.Preparation method of the present invention is simple, repeatability is strong, the existence of the C produced due to the organic carbon of trace makes non-coherent scattering light intensity reduce, and coherent scattering intensity is more outstanding, thus still has higher colorimetric purity at the non-protein stone structure of uneven surface short range order.Not only solve chemical organic compounds pigment fugitive color, harmful technical barrier, solve opal structural strict to substrate requirement simultaneously, the skill difficult problems such as film coating environment is harsh.Semi-conductor, sulfide (such as zinc sulphide) material has a lot of excellent performance, can be applied in sewage disposal, and magneto-optic is changed, antibacterial, the aspects such as photonic crystal, and can be prepared to multifunctional material.So far, document is not also had to carry out report to materials such as utilizing inorganic semiconductor oxide compound, sulfide to prepare this shot-range ordered structure look film.
Carbon black in the obtained blue zinc sulphide photonic crystal structure color film of a kind of method of novelty is utilized to be evenly distributed through the present invention, non-angular dependency, good sphericity, uniform particle diameter, has a wide range of applications in display material, sensing, catalysis and various types of materials surface colour field.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of embodiment 1 gained;
Fig. 2 is the scanning electron microscope (SEM) photograph of embodiment 1 gained;
Fig. 3 is the EDS figure of zinc sulphide microballoon after calcining;
Fig. 4 is the optical photograph of the schemochrome film of embodiment 1 gained;
Fig. 5 amplifies 30 times of photos under the schemochrome Film Optics microscope of embodiment 1 gained.
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
The present invention is achieved through the following technical solutions:
A preparation method for blue zinc sulphide schemochrome colorant, comprises the following steps:
1) in mass ratio for 3:1 takes Zn (NO
3)
26H
2o and polyvinylpyrrolidone (PVP) some grams, add in beaker, proportionally 0.06gPVP:100mL deionized water, and total Water is that 100mL magnetic agitation is fully dissolved and Homogeneous phase mixing, stirs 30min and obtains homogeneous solution;
2) precise thioacetamide 0.3g, adds the ultrasonic mixing 10 ~ 20min of 50mL deionized water, obtains thioacetyl amine aqueous solution;
3) by above-mentioned 1) and 2) after two homogeneous solutions stir respectively, add in same beaker, magnetic agitation 80 DEG C of Water Under bath reaction 6h, the emulsion containing zinc sulphide microballoon can be obtained, then obtain the ethanolic soln of monodisperse ZnS microballoon through ultrasonic disperse after washing, alcohol wash each three are taken second place.
4) glass or ceramic substrate are positioned over step 3) obtained by the ethanolic soln of monodisperse ZnS microballoon dry in 60 DEG C of vacuum drying ovens; obtained short distance word order zinc sulfide film; then by film under nitrogen protection through 300 DEG C of thermal treatments; non-angular dependency can be obtained, the equally distributed blue zinc sulphide photonic crystal structure color film of carbon black.
The sample of the blue zinc sulphide schemochrome film obtained through the present embodiment as shown in Figure 4, Figure 5, can be known and find out that it presents blueness.Its XRD analysis 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, zinc sulphide microsphere surface is coarse for scanning electron microscope (SEM) photograph, height single dispersing, uniform particle diameter (230 ± 10nm).Energy spectrum analysis as shown in Figure 3, as can be seen from the figure except the peak of Zn and S, have also appeared the characteristic peak of C element, show the C element also having trace in ZnS microballoon, and as can be seen from SEM figure, C element is uniformly distributed in mono-dispersion microballoon, and soilless sticking phenomenon occurs.
Embodiment 2
1) in mass ratio for 3.5:1 takes Zn (NO
3)
26H
2o and polyvinylpyrrolidone (PVP) some grams, add in beaker, proportionally 0.055gPVP:100mL deionized water, and total Water is that 100mL magnetic agitation is fully dissolved and Homogeneous phase mixing, stirs 30min and obtains homogeneous solution;
2) precise thioacetamide 0.3g, adds the ultrasonic mixing 10 ~ 20min of 50mL deionized water, obtains thioacetyl amine aqueous solution;
3) by above-mentioned 1) and 2) after two homogeneous solutions stir respectively, add in same beaker, magnetic agitation 80 DEG C of Water Unders bath reaction 7h, can obtain the 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) glass or ceramic substrate are positioned over step 3) obtained by the ethanolic soln of monodisperse ZnS microballoon dry in 50 DEG C of vacuum drying ovens; then by film under nitrogen protection through 500 DEG C of thermal treatments; can obtain low angle dependency, carbon black is uniformly distributed blue zinc sulphide schemochrome film.
Embodiment 3
1) in mass ratio for 4:1 takes Zn (NO
3)
26H
2o and polyvinylpyrrolidone (PVP) some grams, add in beaker, proportionally 0.05gPVP:100mL deionized water, and total Water is that 100mL magnetic agitation is fully dissolved and Homogeneous phase mixing, stirs 30min and obtains homogeneous solution;
2) precise thioacetamide 0.4g, adds the ultrasonic mixing 10 ~ 20min of 50mL deionized water, obtains thioacetyl amine aqueous solution;
3) by above-mentioned 1) and 2) after two homogeneous solutions stir respectively, add in same beaker, magnetic agitation 85 DEG C of Water Unders bath reaction 5h, can obtain the 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) glass or ceramic substrate are positioned over step 3) obtained by the ethanolic soln of monodisperse ZnS microballoon dry in 55 DEG C of vacuum drying ovens; then by film under nitrogen protection through 400 DEG C of thermal treatments; can obtain low angle dependency, carbon black is uniformly distributed blue zinc sulphide schemochrome film.
Embodiment 4
1) in mass ratio for 5:1 takes Zn (NO
3)
26H
2o and polyvinylpyrrolidone (PVP) some grams, add in beaker, proportionally 0.05gPVP:100mL deionized water, and total Water is that 100mL magnetic agitation is fully dissolved and Homogeneous phase mixing, stirs 30min and obtains homogeneous solution;
2) precise thioacetamide 0.5g, adds the ultrasonic mixing 10 ~ 20min of 50mL deionized water, obtains thioacetyl amine aqueous solution;
3) by above-mentioned 1) and 2) after two homogeneous solutions stir respectively, add in same beaker, magnetic agitation 75 DEG C of Water Unders bath reaction 6h, can obtain the 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) glass or ceramic substrate are positioned over step 3) obtained by the ethanolic soln of monodisperse ZnS microballoon dry in 50 DEG C of vacuum drying ovens and obtain short range order zinc sulfide film; then by film under nitrogen protection through 350 DEG C of thermal treatments; can obtain low angle dependency, carbon black is uniformly distributed zinc sulphide blue powder pigment.
In sum, the preparation method of a kind of blue low angle dependency zinc sulphide schemochrome film disclosed by the invention, comprises the preparation of nano-zinc sulfide microballoon; The preparation of shot-range ordered structure look film, by zinc sulfide film calcining under reducing atmosphere; Finally obtain a kind of blue schemochrome film without changeable colors along with angle.The method is with low cost, simple, is applicable at various material surface construction without changeable colors along with angle schemochrome colorant, and preparation method is simple, and repeatability is strong, is easy to extensive preparation.By controlling the particle diameter of microballoon, the multiple colors such as bluish-green, royal purple, purplish blue can be obtained, have a wide range of applications in display material, sensing, catalysis and various types of materials surface colour field.
Claims (7)
1. a preparation method for the blue zinc sulphide photonic crystal structure color film of low angle dependency, is characterized in that, comprise the following steps:
1) by (3 ~ 5): the mass ratio of 1 gets Zn (NO
3)
26H
2o and polyvinylpyrrolidone, then in polyvinylpyrrolidone: the ratio of deionized water=(0.05 ~ 0.06) g:100mL adds deionized water, fully mixes, obtains homogeneous solution;
2) in the ratio of (0.3 ~ 0.5) g:50mL, thioacetamide is dissolved in deionized water, ultrasonic combination treatment, obtains thioacetyl amine aqueous solution;
3) by step 1) obtained homogeneous solution and step 2) obtained thioacetyl amine aqueous solution presses (2 ~ 2.5): after the volume ratio of 1 mixes, at 70 ~ 85 DEG C, water-bath 5 ~ 8h, the obtained emulsion containing zinc sulphide microballoon, again through washing and ultrasonic disperse, the ethanolic soln of obtained monodisperse ZnS microballoon;
4) substrate is placed in the vacuum-drying of monodisperse ZnS microballoon ethanolic soln, obtained zinc sulfide film, by zinc sulfide film under protective atmosphere, through 300 ~ 500 DEG C of calcination processing, obtained blue zinc sulphide photonic crystal structure color colorant.
2. the preparation method of the blue zinc sulphide photonic crystal structure color film of low angle dependency according to claim 1, is characterized in that, step 1) fully to mix be adopt magnetic stirrer 25 ~ 30min.
3. the preparation method of the blue zinc sulphide photonic crystal structure color film of low angle dependency according to claim 1, is characterized in that, step 2) in the ultrasonic combination treatment time be 10 ~ 20min.
4. the preparation method of the blue zinc sulphide photonic crystal structure color film of low angle dependency according to claim 1, it is characterized in that, step 3) described in washing be by the emulsion containing zinc sulphide microballoon first through deionization washing 2 ~ 4 times, then through washes of absolute alcohol 2 ~ 4 times.
5. the preparation method of the blue zinc sulphide photonic crystal structure color film of low angle dependency according to claim 1, is characterized in that, step 4) described protective atmosphere adopts nitrogen or argon gas.
6. the preparation method of the blue zinc sulphide photonic crystal structure color film of low angle dependency according to claim 1, is characterized in that, step 4) described vacuum-drying carries out at 50 ~ 65 DEG C.
7. the blue zinc sulphide photonic crystal structure color film of low angle dependency adopting the method in claim 1 ~ 6 described in any one obtained, it is characterized in that, this low angle dependency blue zinc sulphide photonic crystal structure color film carbon black is evenly distributed, non-angular dependency, good sphericity, uniform particle diameter.
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| CN105694085A (en) * | 2016-02-03 | 2016-06-22 | 陕西科技大学 | Method for lowering color generation angle dependency of PS colloidal crystal film |
| US10649113B2 (en) | 2017-09-29 | 2020-05-12 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
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| CN105694085A (en) * | 2016-02-03 | 2016-06-22 | 陕西科技大学 | Method for lowering color generation angle dependency of PS colloidal crystal film |
| US11385382B2 (en) | 2017-09-29 | 2022-07-12 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
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| US11112537B2 (en) | 2017-09-29 | 2021-09-07 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
| US11131791B2 (en) | 2017-09-29 | 2021-09-28 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
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| US11609359B2 (en) | 2017-09-29 | 2023-03-21 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
| US10649113B2 (en) | 2017-09-29 | 2020-05-12 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
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| US10928552B2 (en) | 2017-09-29 | 2021-02-23 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
| US11402544B2 (en) | 2017-09-29 | 2022-08-02 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
| US11402545B2 (en) | 2017-09-29 | 2022-08-02 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
| US11597996B2 (en) | 2019-06-26 | 2023-03-07 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
| US11840755B2 (en) | 2019-06-26 | 2023-12-12 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
| US11612208B2 (en) | 2019-07-26 | 2023-03-28 | Nike, Inc. | Structurally-colored articles and methods for making and using structurally-colored articles |
| US11412817B2 (en) | 2020-08-07 | 2022-08-16 | Nike, Inc. | Footwear article having repurposed material with concealing layer |
| US11241062B1 (en) | 2020-08-07 | 2022-02-08 | Nike, Inc. | Footwear article having repurposed material with structural-color concealing layer |
| US11129444B1 (en) | 2020-08-07 | 2021-09-28 | Nike, Inc. | Footwear article having repurposed material with concealing layer |
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