CN105174302B - Red low-angle-dependence zinc sulfide structure color materials and preparation method thereof - Google Patents
Red low-angle-dependence zinc sulfide structure color materials and preparation method thereof Download PDFInfo
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- CN105174302B CN105174302B CN201510604483.0A CN201510604483A CN105174302B CN 105174302 B CN105174302 B CN 105174302B CN 201510604483 A CN201510604483 A CN 201510604483A CN 105174302 B CN105174302 B CN 105174302B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses red low-angle-dependence zinc sulfide structure color materials and a preparation method thereof, and belongs to the technical field of photonic crystal material preparation. The preparation method comprises the steps that firstly, zinc sulfide microsphere nanoparticles with the uniform particle size are prepared by adopting a chemical homogeneous precipitation method; secondly, the zinc sulfide microsphere nanoparticles are calcinated under protection of a reducing atmosphere to carbonize trace organic substances, and then the red structure color materials with carbon black evenly distributed are obtained. According to the red low-angle-dependence zinc sulfide structure color materials and the preparation method thereof, the preparation method is simple and high in repeatability, and the technical problems that chemical organic substance color materials are prone to discoloring and harmful to a human body are solved; the technology operation process is simple and easy to operate, large-scale industrial production can be achieved, the method is suitable for construction of angle-free different-color structure color materials on the surfaces of various materials, and the wide application prospect is achieved; the prepared red zinc sulfide photonic crystal structure color materials are even in carbon black distribution, free of angle dependence, good in sphericity degree and uniform in particle size and have the wide application prospect on the fields of material displaying, sensing, catalyzing, various material surface coloring and the like.
Description
Technical field
The invention belongs to schemochrome technical field of material is and in particular to a kind of low angle dependence redness zinc sulphide is tied
Structure color colorant and preparation method thereof.
Background technology
The materials arranged in alternating of high low-refraction forms periodic structure-photonic crystal, thus the light of specific wavelength is not
The photon band gap that can be produced by it, thus create schemochrome.Schemochrome is a kind of physics colour generation, has bright-colored, forever
The advantages of colour-fast, environmental friendliness, short preparation period.Passed through the orderly self-assembly method of colloid micro ball in the last few years, and can be formed
Photonic crystal of opals structure, last light have periodic structure photon crystal surface formed by dry penetrate, diffraction, dissipate
The effect of penetrating etc., thus producing bright and colourful schemochrome, but is because with rainbow effect, the color that is, different directions are observed
Difference, thus greatly limit schemochrome in FPD, the application of the aspect such as printed medium and optical device.Generally, make
Standby photonic crystal powder state typically presents white.By after being assembled into orderly photon crystal film could be in only
Reveal schemochrome (cn103288491a, cn103288492a).Also there is researcher to propose the micro black pigment of interpolation can improve
Color saturation, and can effectively reduce the dependence to angle for the schemochrome, reach and protect with viewing angle change schemochrome
Hold constant effect (cn103173039a, 102702791a, 103788770a), but said method is disadvantageous in that, light
In sub- crystal structure color film preparation, need for powder to mix masking with micro carbon black or black pigment, technique is more complicated, and
Opal structural is very high to film coating environment requirement, and big by external environmental interference, the environmental fluctuating of very little all can be to the quality of film
Have a great impact, be therefore difficult to be widely used.Many researchers add in silica or polystyrene colloidal liquid solution
Micro carbon black or melanin, prepare shortrange order, the schemochrome film of longrange disorder, wherein charcoal using methods such as spin coatings
Black or melanic effect is can there is stronger absorption in visible light wave range, thus reduce incoherent scattering so that
Schemochrome film also can show higher color saturation in the state of shortrange order, longrange disorder, simultaneously this short
Cheng Youxu, the structure of longrange disorder, because isotropism, has low angle dependence, that is, with the change of viewing angle,
Color is basically unchanged, and can be applied to show, the aspect such as printing.But, the ultrafine nanometer carbon black tool applied in this process
There is higher surface energy, the shortcomings of therefore there is difficult dispersion, easily reunite, and be difficult to dissolving in most solution, and Organic Black
Color dyestuff needs to carry out the technical process such as colorant match, colour mixture, and process is complicated and organic black dyes that prepare is unstable etc. lacks
Point.
In the last few years, semiconductor sulfide (such as zinc sulphide) material had much excellent performance such as in sewage because of it
Process, magneto-optic is changed, antibacterial, and the aspect such as photonic crystal receives significant attention.But, so far, also there is no document to utilization
The materials such as sulfide carried out report the preparation to prepare this shot-range ordered structure high saturation mechanism colour glaze.
Content of the invention
For the defect overcoming above-mentioned prior art to exist, it is an object of the invention to provide a kind of low angle dependence is red
Color zinc sulphide schemochrome colorant and preparation method thereof, the method is simple to operate, and repeatability is strong, suitable industrial-scale production；Warp
The prepared spherical zine sulfide photonic crystal of the method is spherical to spend, and uniform particle diameter is widely used.
The present invention is to be achieved through the following technical solutions:
The invention discloses a kind of preparation method of low angle dependence redness zinc sulphide schemochrome colorant, walk including following
Rapid:
1) (10～12) are pressed: 1 mass ratio takes zn (no3)2·6h2O and polyvinylpyrrolidone, by polyvinylpyrrolidine
Ketone: the ratio of deionized water=(0.02～0.03) g:100ml adds deionized water, is sufficiently mixed uniformly, obtains homogeneous solution；
2) in the ratio of (0.3～0.5) g:50ml, thioacetamide is dissolved in deionized water, ultrasonic mixing is processed, and obtains
To thioacetyl amine aqueous solution；
3) by step 1) homogeneous solution and the step 2 that are obtained) the thioacetyl amine aqueous solution that is obtained press 2:1 volume ratio mixed
After even, at 70～85 DEG C, water-bath 5～8h, emulsion containing zinc sulphide microballoon is obtained, then passes through washing and ultrasonic point
Dissipate, the ethanol solution of prepared monodisperse ZnS microballoon；
4) monodisperse ZnS microballoon ethanol solution is vacuum dried, prepared powder, by powder under protective atmosphere, warp
300～500 DEG C of calcination processing, prepared low angle dependence redness zinc sulphide schemochrome colorant.
Step 1) to be sufficiently mixed be uniformly using magnetic stirrer 25～40min.
Step 2) in ultrasonic mixing process time be 10～20min.
Step 3) described in washing be that the emulsion containing zinc sulphide microballoon is first washed 2～4 times through deionization, then through no
Water-ethanol cleans 2～4 times.
Step 4) described protective atmosphere adopt nitrogen or argon gas.
Step 4) described vacuum drying is to carry out at 45～55 DEG C.
The invention also discloses the low angle dependence redness zinc sulphide schemochrome color being obtained using method disclosed above
Material, this red zinc sulphide schemochrome colorant carbon black is evenly distributed, non-angular dependence, good sphericity, uniform particle diameter.
Compared with prior art, the present invention has a following beneficial technique effect:
The preparation method of low angle dependence redness zinc sulphide schemochrome colorant disclosed by the invention, first adopts chemical homogeneous
The precipitation method, control zn (no by strict3)2·6h2The reaction ratio (10～12:1) of o and polyvinylpyrrolidone, and go from
The consumption of sub- water, prepares the zinc sulphide microsphere nano particle of uniform particle diameter, is then calcined under protective atmosphere, make micro
Organic matter carbonizing, thus obtain carbon black equally distributed redness structure colorant, the face of this carbon containing zinc sulphide microballoon powder pigment
Color will not change with the change of viewing angle, in colour-stable, not fugitive color.Preparation method of the present invention is simple, and repeatability is strong, by
Presence in c produced by micro organic carbon makes incoherent scattering luminous intensity reduce, and coherent scattering intensity is more
Prominent, thus the non-protein stone structure in rough surface shortrange order still has higher color saturation.Not only solve
Chemical organic compounds pigment fugitive color, harmful technical barrier, solve chemical organic compounds pigment fugitive color, human body is had
The technical barrier of evil, solves opal structural to substrate requirement strictly, the skill difficult problem such as film coating environment harshness simultaneously.Work of the present invention
Skill operating process is simple, can large-scale industrial production it is adaptable in various material surface construction no changeable colors along with angle schemochrome
Colorant, has broad application prospects.
It is evenly distributed through the low angle dependence redness zinc sulphide schemochrome colorant carbon black that the inventive method is obtained, non-angular
Dependence, good sphericity, uniform particle diameter, have extensively in display material, sensing, catalysis and various types of materials surface coloring field
Application prospect.
Brief description
Fig. 1 is the X-ray diffraction pattern of embodiment 1 gained；
Fig. 2 is the scanning electron microscope (SEM) photograph of embodiment 1 gained；
Fig. 3 eds figure after calcining for zinc sulphide microballoon；
Fig. 4 is the optical photograph of the schemochrome film of embodiment 1 gained.
Fig. 5 is the optical photograph of 20 times of amplification under the microscope of schemochrome powder applying example 1 gained.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, described be explanation of the invention and
It is not to limit.
Embodiment 1
The present invention is to be achieved through the following technical solutions:
A kind of preparation method of low angle dependence redness zinc sulphide schemochrome colorant, comprises the following steps:
1) weigh zn (no for 10:1 in mass ratio3)2·6h2O and some grams of polyvinylpyrrolidone (pvp), add beaker
In, proportionally 0.03g pvp:100ml deionized water, total Water fully dissolves and uniformly mixes for 100ml magnetic agitation, stirs
Mix 30min and obtain homogeneous solution；
2) some 0.3g of precise thioacetamide, plus 50ml deionized water ultrasonic mixing 10～20min, obtains thio
Acetyl amine aqueous solution；
3) by above-mentioned 1) and 2) after two homogeneous solutions stir respectively, add in same beaker, magnetic agitation 80
Water-bath 6h under the conditions of DEG C, you can obtain the emulsion containing zinc sulphide microballoon, then through washing, alcohol wash each three take second place after through
Ultrasonic disperse obtains the ethanol solution of monodisperse ZnS microballoon.
4) by step 3) obtained by the ethanol solution of monodisperse ZnS microballoon dry in 60 DEG C of vacuum drying chambers, system
Obtain powder, then powder is heat-treated through 300 DEG C under nitrogen protection, you can obtain non-angular dependence, carbon black uniformly divides
The red zinc sulphide schemochrome colorant of cloth.
Through the present embodiment be obtained low angle dependence redness zinc sulphide schemochrome colorant sample as shown in Figure 4 and Figure 5,
It is clear that it assumes redness.As shown in figure 1,2 θ=28.2 °, 47.7 °, 56.6 ° correspond to zns's respectively for its xrd analysis
(111), (220), (311) crystal face, and in addition to zns characteristic peak, do not have other miscellaneous peaks to occur, show prepared sample
For pure zns.；Scanning electron microscope (SEM) photograph is as shown in Fig. 2 it can be seen that photon crystal surface is coarse, zinc sulphide microballoon is high
Degree single dispersing, uniform particle diameter (300 ± 10nm) and it can be seen that c element is uniformly distributed in mono-dispersion microballoon, no
Agglomeration occurs..Energy spectrum analysis is as shown in figure 3, as can be seen from the figure have also appeared c element in addition to the peak of zn and s
Characteristic peak, show to also have micro c element in zns microballoon.
Embodiment 2
1) weigh zn (no for 11:1 in mass ratio3)2·6h2O and some grams of polyvinylpyrrolidone (pvp), add beaker
In, proportionally 0.02g pvp:100ml deionized water, total Water fully dissolves and uniformly mixes for 100ml magnetic agitation, stirs
Mix 30min and obtain homogeneous solution；
2) some 0.3g of precise thioacetamide, plus 50ml deionized water ultrasonic mixing 10～20min, obtains thio
Acetyl amine aqueous solution；
3) by above-mentioned 1) and 2) after two homogeneous solutions stir respectively, add in same beaker, magnetic agitation 70
Water-bath 8h under the conditions of DEG C, you can obtain the emulsion containing zinc sulphide microballoon.Through washing, alcohol wash each three take second place after through super
Sound dispersion obtains the ethanol solution of monodisperse ZnS microballoon；
4) by step 3) obtained by the ethanol solution of monodisperse ZnS microballoon dry in 50 DEG C of vacuum drying chambers, so
Afterwards powder is heat-treated through 500 DEG C under nitrogen protection, you can obtain low angle dependence, it is red that carbon black is uniformly distributed zinc sulphide
Color powder pigment.
Embodiment 3
1) weigh zn (no for 12:1 in mass ratio3)2·6h2O and some grams of polyvinylpyrrolidone (pvp), add beaker
In, proportionally 0.03g pvp:100ml deionized water, total Water fully dissolves and uniformly mixes for 100ml magnetic agitation, stirs
Mix 30min and obtain homogeneous solution；
2) some 0.4g of precise thioacetamide, plus 50ml deionized water ultrasonic mixing 10～20min, obtains thio
Acetyl amine aqueous solution；
3) by above-mentioned 1) and 2) after two homogeneous solutions stir respectively, add in same beaker, magnetic agitation 85
Water-bath 5h under the conditions of DEG C, you can obtain the emulsion containing zinc sulphide microballoon.Through washing, alcohol wash each three take second place after through super
Sound dispersion obtains the ethanol solution of monodisperse ZnS microballoon；
4) by step 3) obtained by the ethanol solution of monodisperse ZnS microballoon dry in 45 DEG C of vacuum drying chambers, so
Afterwards powder is heat-treated through 400 DEG C under nitrogen protection, you can obtain non-angular dependence, it is red that carbon black is uniformly distributed zinc sulphide
Color powder pigment.
Embodiment 4
1) weigh zn (no for 10:1 in mass ratio3)2·6h2O and some grams of polyvinylpyrrolidone (pvp), add beaker
In, proportionally 0.02g pvp:100ml deionized water, total Water fully dissolves and uniformly mixes for 100ml magnetic agitation, stirs
Mix 30min and obtain homogeneous solution；
2) some 0.5g of precise thioacetamide, plus 50ml deionized water ultrasonic mixing 10～20min, obtains thio
Acetyl amine aqueous solution；
3) by above-mentioned 1) and 2) after two homogeneous solutions stir respectively, add in same beaker, magnetic agitation 75
Water-bath 6h under the conditions of DEG C, you can obtain the emulsion containing zinc sulphide microballoon.Through washing, alcohol wash each three take second place after through super
Sound dispersion obtains the ethanol solution of monodisperse ZnS microballoon；
4) by step 3) obtained by the ethanol solution of monodisperse ZnS microballoon dry in 55 DEG C of vacuum drying chambers, so
Afterwards powder is heat-treated through 350 DEG C under nitrogen protection, you can obtain non-angular dependence, it is red that carbon black is uniformly distributed zinc sulphide
Color powder pigment.
In sum, the preparation method of a kind of redness zinc sulphide photonic crystal structure color colorant disclosed by the invention, including
The preparation of nano-zinc sulfide microballoon；By the calcining under zinc sulphide micro-sphere material reducing atmosphere；Finally give one kind no changeable colors along with angle
Red schemochrome colorant.The method with low cost, simple it is adaptable to various material surface construction no changeable colors along with angle knot
Structure color colorant, and preparation method is simple, repeatability is strong it is easy to extensive prepare.By controlling the particle diameter of microballoon, indigo plant can be obtained
Green, royal purple, the multiple color such as purplish red, have widely in display material, sensing, catalysis and various types of materials surface coloring field
Application prospect.
Claims (5)
1. a kind of preparation method of redness low angle dependence zinc sulphide schemochrome colorant is it is characterised in that comprise the following steps:
1) (10～12) are pressed: 1 mass ratio takes zn (no3)2·6h2O and polyvinylpyrrolidone, by polyvinylpyrrolidone: go
The ratio of ionized water=(0.02～0.03) g:100ml adds deionized water, is sufficiently mixed uniformly, obtains homogeneous solution；Fully mixed
Closing is uniformly using magnetic stirrer 25～40min；
2) in the ratio of (0.3～0.5) g:50ml, thioacetamide is dissolved in deionized water, ultrasonic mixing process 10～
20min, obtains thioacetyl amine aqueous solution；
3) by step 1) homogeneous solution and the step 2 that are obtained) the thioacetyl amine aqueous solution that is obtained press the volume ratio mixing of 2:1
Afterwards, at 70～85 DEG C, water-bath 5～8h, emulsion containing zinc sulphide microballoon is obtained, then passes through washing and ultrasonic point
Dissipate, the ethanol solution of prepared monodisperse ZnS microballoon；
4) monodisperse ZnS microballoon ethanol solution is vacuum dried, prepared powder, by powder under protective atmosphere, through 300～
500 DEG C of calcination processing, are obtained redness low angle dependence zinc sulphide schemochrome colorant.
2. the preparation method of redness low angle dependence zinc sulphide schemochrome colorant according to claim 1, its feature exists
In step 3) described in washing be that the emulsion containing zinc sulphide microballoon is first washed 2～4 times through deionization, then through anhydrous second
Alcohol cleans 2～4 times.
3. the preparation method of redness low angle dependence zinc sulphide schemochrome colorant according to claim 1, its feature exists
In step 4) described protective atmosphere adopt nitrogen or argon gas.
4. the preparation method of redness low angle dependence zinc sulphide schemochrome colorant according to claim 1, its feature exists
In step 4) described vacuum drying is to carry out at 45～55 DEG C.
5. adopt the red low angle dependence zinc sulphide schemochrome that in Claims 1 to 4, the method described in any one is obtained
Colorant it is characterised in that this red low angle dependence zinc sulphide schemochrome colorant carbon black is evenly distributed, low angle dependence,
Good sphericity, uniform particle diameter.
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| CN110682883A (en) * | 2019-09-10 | 2020-01-14 | 神通科技集团股份有限公司 | Totally-enclosed automobile grille |
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| CN109264768A (en) * | 2018-11-23 | 2019-01-25 | 陕西科技大学 | A kind of low angle dependence green cadmium sulfide schemochrome film and preparation method thereof |
| CN109319825A (en) * | 2018-11-23 | 2019-02-12 | 陕西科技大学 | A kind of low angle dependence purple cadmium sulfide schemochrome film and preparation method thereof |
| CN109485089A (en) * | 2018-11-23 | 2019-03-19 | 陕西科技大学 | A kind of low angle dependence blue cadmium sulfide schemochrome film and preparation method thereof |
| CN109455944A (en) * | 2018-11-23 | 2019-03-12 | 陕西科技大学 | A kind of low angle dependence red cadmium sulfide schemochrome film and preparation method thereof |
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| CN100586863C (en) * | 2008-09-27 | 2010-02-03 | 燕山大学 | Method for controlling micrometre zinc sulphide morphology by Escherichia coli biological template |
| CN102515255A (en) * | 2012-01-09 | 2012-06-27 | 西南大学 | Method for preparing zinc sulfide nanospheres |
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| CN110682883A (en) * | 2019-09-10 | 2020-01-14 | 神通科技集团股份有限公司 | Totally-enclosed automobile grille |
| CN110682883B (en) * | 2019-09-10 | 2021-05-11 | 神通科技集团股份有限公司 | Totally-enclosed automobile grille |
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