CN105111481B - A kind of green photon crystal structure color film with photocatalytic effect and preparation method thereof - Google Patents
A kind of green photon crystal structure color film with photocatalytic effect and preparation method thereof Download PDFInfo
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- CN105111481B CN105111481B CN201510604367.9A CN201510604367A CN105111481B CN 105111481 B CN105111481 B CN 105111481B CN 201510604367 A CN201510604367 A CN 201510604367A CN 105111481 B CN105111481 B CN 105111481B
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- crystal structure
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Abstract
The invention discloses a kind of green photon crystal structure color film with photocatalytic effect and preparation method thereof, belong to photonic crystal structure color film preparing technical field.Use sluggish precipitation first, be prepared for the zinc sulphide microballoon for making uniform particle diameter, then using vertical deposition method in glass basis surface self-organization into green photon crystal structure color film.This schemochrome green film color is beautiful, not fugitive color, solves the shortcomings that chemical organic compounds pigment fugitive color, harmful.And realize photocatalytic degradation function of the photonic crystal structure color film to rhodamine B.Present invention process process is simple and easy, energy large-scale industrial production, has broad application prospects.
Description
Technical field
The invention belongs to photonic crystal structure color film preparing technical field, and in particular to a kind of with photocatalytic effect
The preparation method of green photon crystal structure color film.
Background technology
Photonic crystal is that dielectric refractive index cyclically-varying causes photonic band gap structure, so as to by photonic band gap structure control
Make the motion of light in the photonic crystal.Photonic crystal is that low refraction periodically occur in some positions of high-index material
The material of rate.The materials arranged in alternating of high low-refraction forms periodic structure can and produces photonic band gap.So as to produce
Schemochrome is given birth to.This is a kind of physics colour generation, and it has bright-colored, will never fade, environment-friendly, short preparation period etc. excellent
Point.Wherein pass through the orderly self-assembly method of colloid micro ball, it becomes possible to form photonic crystal of opals structure, have photon band gap special
Sign, when incident light frequency falls in bandgap range, the incident light will not pass through the photonic crystal, and these can not continue to propagate
Visible ray can be reflected by photonic crystal, finally form coherent diffraction in the photon crystal surface with periodic structure, and produce
Raw bright and colourful schemochrome.By to the research in nature with artificial preparation structure color, showing, decorate, preventing at present
There is good application in the fields such as puppet.As Chinese invention patent application CN201310205537.7 discloses a kind of red photon crystal
The preparation method of structure color glaze, mainly obtained by the self-assembling technique of silicon dioxide microsphere on ceramic body surface, should
Red photon crystal structure color has preferable colouring effect.One is disclosed in Chinese invention patent application CN201010276061.2
Plant hydro-thermal method and prepare zinc sulphide microballoon, and announce the zinc sulphide microballoon there is good ultraviolet light response.It is however, right at present
The research of photonic crystal structure color film is only limitted to the imitated and analysis in different colours colouring effect, and main material is then oxygen
The materials such as SiClx, polystyrene, to the photonic crystal structure color material of multifunctionality, particularly to the light with photocatalysis performance
Sub- crystal structure color thin film study is very few.
The content of the invention
It is will never fade it is an object of the invention to provide a kind of bright-colored, and the green light with photocatalytic effect
Sub- crystal structure color film and preparation method thereof.
The present invention is to be achieved through the following technical solutions：
The invention discloses a kind of preparation method of the green photon crystal structure color film with photocatalytic effect, including
Following steps：
1) 9 are pressed:The mass ratio of (1~2), weigh Zn (NO3)2·6H2O and polyvinylpyrrolidone, after mixing, by Zn
(NO3)2·6H2O：Deionized water=(0.3~0.5) g：100mL ratio adds deionized water, stirs, and obtains
Even solution；
2) (0.25~0.4) g is pressed：50mL amount ratio, thioacetamide is added in deionized water, ultrasonic mixing is equal
It is even, obtain thioacetyl amine aqueous solution；
3) by step 1) and 2) made from two solution, by (1~2)：After 1 volume ratio mixing, at 70~85 DEG C, water
5~7h of stirring reaction is bathed, obtains the emulsion containing zinc sulphide microballoon, then is washed through washing, alcohol and ultrasonic disperse is handled, obtains list
The alcoholic solution of dispersed sulfur zinc microballoon；
4) slide by cleaning is disposed vertically in the alcoholic solution of monodisperse ZnS microballoon made from step 3), in 40
At~60 DEG C, after vacuum drying treatment to alcohol volatilization completely, green photon crystal structure color film is generated in slide surface, then
Under nitrogen protection by 300~500 DEG C of heat treatments, the green photon crystal structure color film with photocatalytic effect is made.
Step 1) stirs handles 20~35min using magnetic stirrer.
The ultrasonic mixing time is 10~20min in step 2).
Washing in step 3), alcohol is washed is to clean the emulsion containing zinc sulphide microballoon three times with water and ethanol successively.
The ultrasonic disperse time is 10~20min in step 3).
Clean slide described in step 4) is that slide is placed in into H2SO4With H2O2It is 7 by volume:3 water prepared
In solution, 30min is soaked, is then cleaned with distilled water, dried and be made at 60 DEG C.
The vacuum drying treatment time is 35~45h in step 4).
Heat treatment time is 1~3h in step 4).
The invention also discloses thin using the green photon crystal structure color with photocatalytic effect made from the above method
Film.
Compared with prior art, the present invention has technique effect beneficial below：
The preparation method of green photon crystal structure color film disclosed by the invention with photocatalytic effect, is used first
Sluggish precipitation, by strictly controlling Zn (NO3)2·6H2O and polyvinylpyrrolidone reaction ratio (9：1~2 quality
Than), and the dosage of the deionized water added, the emulsion containing zinc sulphide microballoon is prepared, zinc sulphide microspherulite diameter is
250±10nm；Then using vertical deposition method in glass basis surface self-organization into green photon crystal structure color film.It is this
Schemochrome green film color is beautiful, not fugitive color, solves the shortcomings that chemical organic compounds pigment fugitive color, harmful.
And realize photocatalytic degradation function of the photonic crystal structure color film to rhodamine B.Present invention process process is simple and easy,
Energy large-scale industrial production, has broad application prospects.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram for the green schemochrome film that the gained of embodiment 1 has photocatalytic effect；
Fig. 2 is the reflectance spectrum figure for the green schemochrome film that the gained of embodiment 1 has photocatalytic effect；
Fig. 3 is the rhodamine B photocatalysis for the green photon crystal structure color film that the gained of embodiment 1 has photocatalytic effect
Degraded figure.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
A kind of preparation method of the green photon crystal structure color film with photocatalytic effect, comprises the following steps：
(1) it is 9 in mass ratio：1 weighs Zn (NO3)2·6H2O and some grams of polyvinylpyrrolidone (PVP), add beaker
In, proportionally 0.45gZn (NO3)2 ·6H2O：100mL, adds deionized water, and magnetic agitation fully dissolves and uniformly mixed, stirs
Mix 30min and just obtain homogeneous solution.
(2) precise thioacetamide 0.3g, add 50mL deionized water 10~20min of ultrasonic mixing, obtain thio second
Amide aqueous solution.
(3) after above-mentioned (1) and (2) two solution stirring respectively, add in same beaker, and in magnetic agitation
On instrument under the conditions of 80 DEG C water-bath 6h, you can obtain obtaining emulsion containing zinc sulphide microballoon.Wash each three through washing, alcohol and take second place
Afterwards the ethanol solution of monodisperse ZnS microballoon is obtained by ultrasonic disperse.
(4) slide of a certain size (25.6 × 76.2mm) is placed in H2SO4/H2O2(7:Soaked in aqueous solution 3V/V)
30min is steeped, then takes out and is cleaned with a large amount of distilled water, finally dries, saves backup in 60 DEG C of baking ovens.
The slide cleaned is disposed vertically in the ZnS microballoon emulsion obtained by step 3, and by whole system
It is placed in constant temperature (40~60 DEG C ± 1 DEG C) vacuum drying chamber, approximately passes through 40h, after ethanol volatilization completely, in glass substrate table
Face will generate a kind of green photon crystal structure color film with photocatalytic effect.Pass through 400 DEG C of heat under nitrogen protection
Processing, you can obtain the zinc sulphide photon crystal film with photocatalysis performance.
It is as follows to the method for testing of green photon crystal structure color film color generation property made from the present embodiment：
Analyzed using the reflectance spectrum of ultraviolet-visible-near-infrared spectrum instrument, INSTRUMENT MODEL：The types of Lamda 950, the U.S.
Beckman companies, 175~3300nm of wave-length coverage, 0.5~5.0nm of bandwidth, veiling glare<0.00008%T, wavelength accuracy
0.08nm, scanning three times, are averaged.
The method of testing of Green photonic crystal structure color film photocatalysis performance of the present invention is as follows：
Photocatalytic degradation rhodamine B solution, the rhodamine B solution 40 that concentration is 10mg/L is added in light-catalyzed reaction instrument
The film size that~80ml and step 4) obtain is the 1cm × 2cm orange-yellow photonic crystal structure color with photocatalytic effect
Film, 10min then is reacted in unglazed darkroom, be sufficiently mixed ZnS microballoons and rhodamine B reaction solution, reach absorption/de-
Attached balance.Light-catalyzed reaction opens 500W mercury lamp after starting, and is at the uniform velocity stirred by magnetic stirring apparatus, is sampled every 10min,
The degradation effect of organic matter is determined by the absorbance of reaction solution.Absorbance is to use Lambda-950 type ultraviolet-visible lights
Spectrometer determines.
With the degraded of rhodamine B solution solution that is used for being degraded of initial concentration in the concentration of t and its solution
Rate, characterize the Photocatalytic Degradation Property of ZnS microballoons respectively：
C/C0=A/A0
In formula, C0Represented respectively with C reaction start before solution concentration and photocatalysis start after solution when reacting t times
Concentration, A0Represent that reaction starts the absorbance at the absorbing wavelength that solution is maximum during the preceding and light-catalyzed reaction t times respectively with A
Value.
Through its XRD analysis of the sample of green zinc sulphide photonic crystal structure color film made from the present embodiment as shown in figure 1,
Its XRD analysis is as shown in figure 1,2 θ=28.2 °, 47.7 °, 56.6 ° of (111) for corresponding to ZnS respectively, (220), (311) crystal face, and
And in addition to ZnS characteristic peaks, occur without other miscellaneous peaks, show that prepared sample is pure ZnS.；Reflectance spectrum is such as
Shown in Fig. 2, it can be seen that the reflection peak of zinc sulphide schemochrome film is in green fields.Photocatalytic effect is analyzed such as
Shown in Fig. 3, as can be seen from the figure prepared zinc sulphide has good degradation effect to organic dyestuff rhodamine B,
Rhodamine B can just be degraded substantially in 60min complete.
Embodiment 2
A kind of preparation method of the green photon crystal structure color film with photocatalytic effect, comprises the following steps：
(2) it is 9 in mass ratio：2 weigh Zn (NO3)2·6H2O and some grams of polyvinylpyrrolidone (PVP), add beaker
In, proportionally 0.3gZn (NO3)2 ·6H2O：100mL, adds deionized water, and magnetic agitation fully dissolves and uniformly mixed, stirs
Mix 30min and just obtain homogeneous solution.
(2) precise thioacetamide 0.25g, add 50mL deionized water 10~20min of ultrasonic mixing, obtain thio second
Amide aqueous solution.
(3) after above-mentioned (1) and (2) two solution stirring respectively, add in same beaker, and in magnetic agitation
On instrument under the conditions of 70 DEG C water-bath 7h, you can obtain obtaining emulsion containing zinc sulphide microballoon.Wash each three through washing, alcohol and take second place
Afterwards the ethanol solution of monodisperse ZnS microballoon is obtained by ultrasonic disperse.
(4) slide of a certain size (25.6 × 76.2mm) is placed in H2SO4/H2O2(7:Soaked in aqueous solution 3V/V)
30min is steeped, then takes out and is cleaned with a large amount of distilled water, finally dries, saves backup in 60 DEG C of baking ovens.
The slide cleaned is disposed vertically in the ZnS microballoon emulsion obtained by step 3, and by whole system
It is placed in constant temperature (40~60 DEG C ± 1 DEG C) vacuum drying chamber, approximately passes through 40h, after ethanol volatilization completely, in glass substrate table
Face will generate a kind of green photon crystal structure color film with photocatalytic effect.Pass through 500 DEG C of heat under nitrogen protection
Processing, you can obtain the zinc sulphide photon crystal film with photocatalysis performance.
Embodiment 3
A kind of preparation method of the green photon crystal structure color film with photocatalytic effect, comprises the following steps：
(3) it is 9 in mass ratio：2 weigh Zn (NO3)2·6H2O and some grams of polyvinylpyrrolidone (PVP), add beaker
In, proportionally 0.5gZn (NO3)2 ·6H2O：100mL ratio adds deionized water, and magnetic agitation fully dissolves and uniformly mixed
Close, stirring 30min just obtains homogeneous solution.
(2) precise thioacetamide 0.4g, add 50mL deionized water 10~20min of ultrasonic mixing, obtain thio second
Amide aqueous solution.
(3) after above-mentioned (1) and (2) two solution stirring respectively, add in same beaker, and in magnetic agitation
On instrument under the conditions of 85 DEG C water-bath 5h, you can obtain obtaining emulsion containing zinc sulphide microballoon.Wash each three through washing, alcohol and take second place
Afterwards the ethanol solution of monodisperse ZnS microballoon is obtained by ultrasonic disperse.
(4) slide of a certain size (25.6 × 76.2mm) is placed in H2SO4/H2O2(7:Soaked in aqueous solution 3V/V)
30min is steeped, then takes out and is cleaned with a large amount of distilled water, finally dries, saves backup in 40 DEG C of baking ovens.
The slide cleaned is disposed vertically in the ZnS microballoon emulsion obtained by step 3, and by whole system
It is placed in constant temperature (40~60 DEG C ± 1 DEG C) vacuum drying chamber, approximately passes through 40h, after ethanol volatilization completely, in glass substrate table
Face will generate a kind of green photon crystal structure color film with photocatalytic effect.Pass through 300 DEG C of heat under nitrogen protection
Processing, you can obtain the zinc sulphide photon crystal film with photocatalysis performance.
Claims (6)
- A kind of 1. preparation method of the green photon crystal structure color film with photocatalytic effect, it is characterised in that including with Lower step：1) 9 are pressed:The mass ratio of (1~2), weigh Zn (NO3)2·6H2O and polyvinylpyrrolidone, after mixing, by Zn (NO3)2· 6H2O：Deionized water=(0.3~0.5) g：100mL ratio adds deionized water, stirs, obtains homogeneous solution；2) (0.25~0.4) g is pressed：50mL amount ratio, thioacetamide is added in deionized water, ultrasonic mixing is uniform, obtains To thioacetyl amine aqueous solution；3) by step 1) and 2) made from two solution, by (1~2)：After 1 volume ratio mixing, at 70~85 DEG C, water-bath is stirred 5~7h of reaction is mixed, obtains the emulsion containing zinc sulphide microballoon, then is washed through washing, alcohol and ultrasonic disperse is handled, obtains single dispersing The alcoholic solution of zinc sulphide microballoon；4) slide by cleaning is disposed vertically in the alcoholic solution of monodisperse ZnS microballoon made from step 3), in 40~60 At DEG C, after vacuum drying treatment to alcohol volatilization completely, green photon crystal structure color film is generated in slide surface, then in nitrogen By 300~500 DEG C of heat treatments under gas shielded, the green photon crystal structure color film with photocatalytic effect is made；Wherein, step 1) stirs handles 20~35min using magnetic stirrer, in step 2) during ultrasonic mixing Between be 10~20min, the ultrasonic disperse time is 10~20min in step 3).
- 2. the preparation method of the green photon crystal structure color film according to claim 1 with photocatalytic effect, its It is characterised by, washing in step 3), alcohol is washed is to clean the emulsion containing zinc sulphide microballoon three times with water and ethanol successively.
- 3. the preparation method of the green photon crystal structure color film according to claim 1 with photocatalytic effect, its It is characterised by, the clean slide described in step 4) is that slide is placed in into H2SO4With H2O2It is 7 by volume:3 preparations In the aqueous solution, 30min is soaked, is then cleaned with distilled water, dried and be made at 60 DEG C.
- 4. the preparation method of the green photon crystal structure color film according to claim 1 with photocatalytic effect, its It is characterised by, the vacuum drying treatment time is 35~45h in step 4).
- 5. the preparation method of the green photon crystal structure color film according to claim 1 with photocatalytic effect, its It is characterised by, heat treatment time is 1~3h in step 4).
- 6. using the obtained green photon crystal with photocatalytic effect of method described in any one in Claims 1 to 5 Schemochrome film.
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