CN107119327A - A kind of large area for preparing does not ftracture the method for colloid photonic crystal film - Google Patents
A kind of large area for preparing does not ftracture the method for colloid photonic crystal film Download PDFInfo
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- CN107119327A CN107119327A CN201710225398.2A CN201710225398A CN107119327A CN 107119327 A CN107119327 A CN 107119327A CN 201710225398 A CN201710225398 A CN 201710225398A CN 107119327 A CN107119327 A CN 107119327A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/54—Organic compounds
- C30B29/58—Macromolecular compounds
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/002—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
- G02B1/005—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials made of photonic crystals or photonic band gap materials
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Abstract
Do not ftracture the method for colloid photonic crystal film, comprise the following steps that the invention discloses a kind of large area for preparing：Aqueous polyurethane emulsion is distributed in colloidal particle solution；Then using the homogeneous phase solution that is configured to as coating liquid, large area colloid photonic crystal film is scratched out on hydrophobic substrate with silk rod；Again in one layer of quantum dot of surface spin coating of colloid photonic crystal film.Resonance effects using colloidal photon crystal in visible region can significantly increase the fluorescence signal of quantum dot.Instant invention overcomes the shortcoming that traditional colloid photonic crystal film is easy to crack, with simple to operate, mild condition, the advantages of being easy to large-area construction, prepared colloidal photon crystal and quantum dot composite membrane have very high fluorescence intensity and fluorescent stability, can be for quickly preparing high power QD LED components provides thinking.
Description
Technical field
Do not ftractureed the method for colloid photonic crystal film the present invention relates to a kind of large area for preparing, more specifically to utilization
Adhesion between hydrogen bond enhancing colloid micro ball, realizes photonic crystal large area film forming without cracking in polyurethane, and further
For the method for the fluorescence intensity for strengthening quantum dot.
Background technology
Colloidal photon crystal is a kind of by single dispersing organic or inorganic colloidal particle, passes through the new of the preparation of method from bottom to top
Functional material.Due to the periodic arrangement of its spatially long-range order, the feature with forbidden photon band, thus be widely used
In fields such as display, chemical sensitisation and Fluorescence Increasings.At present, how to solve the problem of large area film forming is without cracking turns into photon
The focus of Crystal study.Up to now, the method for the photonic crystal film forming reported has：Vertical deposition method, outfield force induction group
Dress method, template assemblies method etc., but there is complex steps, consuming in these methods, greatly limit Colloidal photonic
The practical application of crystal.And in film forming procedure, when solvent volatilizees, the capillary force between colloid micro ball can produce horizontal pressure
Stress, when this transverse compressive stress exceedes critical value, crackle occurs in the crystal film with photon ultimately formed, and the generation of crackle is seriously limited
It is prepared by the large area for having made colloid photonic crystal film.Therefore, how film forming procedure is solved using easy and effective, inexpensive method
In problem of Cracking prepared by high-performance crystal film with photon to quick big face be particularly important.
In recent years, although LED component experienced the development of abundance, relatively low light extraction efficiency seriously limits LED light
Source power output.Therefore researching and developing high-power LED component turns into the key for widening LED application fields.
The content of the invention
The technical problem to be solved in the present invention is to overcome photonic crystal film formation step complicated, easily cracking, it is difficult to large area
The shortcomings of construction, do not ftractureed the method for colloid photonic crystal film so as to provide a kind of large area for preparing.The method mild condition, step
Rapid simple, reproducible, prepared colloid photonic crystal film has large area, not ftractureed, the characteristics of optical property is excellent.
To reach above-mentioned purpose, contain hydrogen bond network the technical scheme is that being introduced in colloid micro ball emulsion system
Polyaminoester emulsion, by the hydrogen bond action of microballoon and polyurethane network to strengthen adhesion between microballoon, so as to realize large area
Film forming is without ftractureing.The present invention using high optical quality crystal film with photon it is extremely strong Bragg diffraction effect so that photon with
The group velocity of decrease is propagated in the photonic crystal, is reached the effect of the gain of light, that is, is reached the effect of Fluorescence Increasing.
The present invention concrete technical scheme be：A kind of method for preparing colloidal photon crystal and quantum dot composite membrane, it has
Body step is as follows：Aqueous polyurethane is distributed in colloidal particle solution；Then using the homogeneous phase solution that is configured to as coating liquid, use
Silk rod scratches out large area colloid photonic crystal film on hydrophobic substrate；Finally in the surface of colloid photonic crystal film spin coating instrument
Spin coating goes out one layer of quantum dot.
It is preferred that above-mentioned coating liquid is the mixed aqueous solution of colloidal particle and polyurethane；Colloidal particle wherein in coating liquid
Mass concentration is 25%-35%, and the mass concentration of polyurethane is 1%-5%.
It is preferred that above-mentioned colloidal particle is the monodisperse polystyrene colloid microballoon of surface carboxyl modification；Surface carboxyl modification
Monodisperse polystyrene microsphere particle size range 180nm-300nm, single dispersing coefficient be 1%-5%.
It is preferred that the bandgap center position of the colloid photonic crystal film scratched out is located at 510nm-620nm.
Solution used in preferably spun on instrument spin coating is CdTe quantum and PVA mixed aqueous solution, wherein CdTe quantum
Mass fraction in mixed aqueous solution is 0.1%-1%, and mass fractions of the PVA in mixed aqueous solution is 0.5%-2%.
It is preferred that the emission peak of CdTe quantum is between 510nm-620nm.The spin speed of preferably spun on instrument is
1000rpm-2500rpm, the time is 30s-60s.
It is preferred that above-mentioned hydrophobic substrate is one kind in glass, silicon chip or plastics.It is preferred that the contact of described hydrophobic substrate
Angle is 10 ° -25 °.
Beneficial effect：
1st, colloid photonic crystal film prepared by the present invention has flexible, not easy to crack physical property, and schemochrome is gorgeous, prohibit
The adjustable optical property in band position.
2nd, colloid photonic crystal film prepared by the present invention, which has, is easy to large-area construction, the spy with prospects for commercial application
Point.
3rd, the quantum dot film fluorescence property based on colloidal photon crystal that prepared by the present invention is excellent, and stability is good, and fluorescence is strong
Degree is significantly increased than common quantum dot film.
4th, the quantum dot film based on colloidal photon crystal prepared by the present invention can be efficiently applied to light as fluorophor
In device.
Brief description of the drawings
Fig. 1 is the pictorial diagram of the colloid photonic crystal film of the embodiment of the present invention 1；
Fig. 2 is the Electronic Speculum surface sweeping figure of the colloid photonic crystal film of the embodiment of the present invention 1；
Fig. 3 is the colloid photonic crystal film reflectance spectrum figure of the embodiment of the present invention 1；
Fig. 4 is that the colloidal photon crystal of the embodiment of the present invention 1 strengthens the fluorogram of quantum dot film；
Fig. 5 is fluorescence spectra of the quantum dot film of the embodiment of the present invention 1 under different base, wherein, curve a is not ftracture
Colloid photonic crystal film be background quantum dot fluorescence spectrum, b be cracking colloid photonic crystal film be background quantum dot
Fluorescence spectrum, c is the quantum dot fluorescence spectrogram of film forming in PET.
Embodiment
Illustrate the present invention below by way of specific embodiment, but the present invention is not merely defined in these embodiments.
Embodiment 1
In particle diameter is 228nm, monodisperse polystyrene microsphere emulsion of the single dispersing coefficient for 1% surface carboxyl modification
Polyaminoester emulsion is added, the mixed solution being made, wherein polystyrene microsphere mass fraction are 30%, and polyurethane mass fraction is
1%.Ultrasonic disperse is uniform, until bubble-free.Then scratched, treated for 18 ° of PET film surface in contact angle with silk rod
Solvent seasoning, can obtain indehiscent crystal film with photon.
Fig. 1 is described crystal film with photon pictorial diagram, and size is 30*40cm, and crystal film with photon shows beautiful green knot
Structure color, surface is uniformly without cracking phenomena.
The crystal film with photon is subjected to electron-microscope scanning, as a result referring to Fig. 2, as a result show prepared crystal film with photon by
Monodisperse colloid particle is constituted, and is the close-packed arrays of shortrange order.
Fig. 3 is the reflectance spectrum figure of described crystal film with photon, and the forbidden photon band of crystal film with photon is located at 540nm, half-peak
Wide 30nm, reflected intensity is high.
Aqueous phase CdTe (emission peak 540nm) is added in the PVA aqueous solution, is made in mixed solution, mixed solution, CdTe matter
It is 0.5% to measure the mass fraction that fraction is 0.1%, PVA.
CdTe/PVA solution is added dropwise on bandgap center position 540nm colloid photonic crystal film, with 1200rpm speed spin coating
30s。
Treat that solvent volatilizees, quantum dot film enhanced to colloidal photon crystal carries out solid fluorescence test.
Fig. 5 is the fluorescence spectra of the enhanced quantum dot of colloidal photon crystal that do not ftracture.Wherein, curve a is not open
The colloid photonic crystal film split is the quantum dot fluorescence spectrum of background, and b is that the colloid photonic crystal film of cracking is the quantum of background
Point fluorescence spectrum, c is the quantum dot fluorescence spectrogram of film forming in PET.It can be seen that the Colloidal photonic for being not added with polyurethane is brilliant
Body film makes CdTe quantum fluorescence intensity add one times, and adding after polyurethane the colloid photonic crystal film that do not ftracture makes CdTe amounts
Son point fluorescence intensity adds three times.The fluorescence spectra illustrates that prepared by the present invention does not ftracture colloid photonic crystal film in amount
It is more efficient in son point enhancement effect of fluorescence.
Embodiment 2
It is 211nm in particle diameter, single dispersing coefficient is addition in the monodisperse polystyrene microsphere of 3% surface carboxyl modification
In polyaminoester emulsion, the mixed solution being made, polystyrene microsphere mass fraction is 35%, and polyurethane mass fraction is 3%.It is super
Sound is uniformly dispersed, until bubble-free.Then scratched with silk rod in contact angle for 13 ° of glass surface, treat solvent seasoning, can
To obtain indehiscent crystal film with photon.
Aqueous phase CdTe (emission peak 500nm) is added in concentration is the 1% PVA aqueous solution, mixed solution is made, is mixed molten
In liquid, the mass fraction that CdTe mass fractions are 0.5%, PVA is 1%.CdTe/PVA is added dropwise on colloid photonic crystal film molten
Liquid, with 1500rpm speed spin coating 45s.
Obtained crystal film with photon size is 35*42cm, and reflectance spectrum test is carried out to gained colloid photonic crystal film,
Its bandgap center position is measured positioned at 500nm, fluorescence spectrum test is carried out to gained photonic crystal/quantum dot composite membrane, its is measured glimmering
Light emitting peak is located at 502nm.Contrast original quantum dot film to find, fluorescence intensity has larger enhancing.As a result show, prepared by the present invention
Crystal film with photon there is good enhancement effect of fluorescence for quantum dot film.
Embodiment 3
It is 256nm in particle diameter, single dispersing coefficient is addition in the monodisperse polystyrene microsphere of 5% surface carboxyl modification
In polyaminoester emulsion, the mixed solution being made, polystyrene microsphere mass fraction is 25%, and polyurethane mass fraction is 5%.It is super
Sound is uniformly dispersed, until bubble-free.Then scratched with silk rod in contact angle for 24 ° of silicon chip surface, treat solvent seasoning, can
To obtain indehiscent crystal film with photon.
Aqueous phase CdTe (emission peak 610nm) is added in concentration is the 1.5% PVA aqueous solution, mixed solution is made.Mixing
In solution, the mass fraction that CdTe mass fractions are 1%, PVA is 1.5%.In bandgap center position 610nm colloid photonic crystal film
Upper dropwise addition CdTe/PVA solution, with 2000rpm speed spin coating 60s.
Obtained crystal film with photon size is 32*41cm, and reflectance spectrum test is carried out to gained colloid photonic crystal film,
Its bandgap center position is measured positioned at 606nm, fluorescence spectrum test is carried out to gained photonic crystal/quantum dot composite membrane, its is measured glimmering
Light emitting peak is located at 610nm.Contrast original quantum dot film to find, fluorescence intensity has larger enhancing.As a result show, prepared by the present invention
Crystal film with photon there is good enhancement effect of fluorescence for quantum dot film.
Claims (9)
1. a kind of large area for preparing does not ftracture the method for colloid photonic crystal film, it is comprised the following steps that：By aqueous polyurethane point
It is scattered in colloidal particle solution；Then using the homogeneous phase solution that is configured to as coating liquid, plastic emitting is scratched on hydrophobic substrate with silk rod
Body crystal film with photon；The last surface spin coating instrument spin coating in colloid photonic crystal film goes out one layer of quantum dot.
2. according to the method described in claim 1, it is characterised in that described coating liquid is the mixing of colloidal particle and polyurethane
The aqueous solution；The mass concentration of colloidal particle is 25%-35% wherein in coating liquid, and the mass concentration of polyurethane is 1%-5%.
3. according to the method described in claim 1, it is characterised in that described colloidal particle is the single dispersing of surface carboxyl modification
Polystyrene colloid microballoon；The particle size range 180nm-300nm of the monodisperse polystyrene microsphere of surface carboxyl modification, single dispersing
Coefficient is 1%-5%.
4. according to the method described in claim 1, it is characterised in that the bandgap center position position of the colloid photonic crystal film scratched out
In 510nm-620nm.
5. according to the method described in claim 1, it is characterised in that the solution used in spin coating instrument spin coating is CdTe quantum and PVA
Mixed aqueous solution, wherein mass fraction of the CdTe quantum in mixed aqueous solution be 0.1%-1%, PVA mix it is water-soluble
Mass fraction in liquid is 0.5%-2%.
6. according to the method described in claim 1, it is characterised in that the emission peak of CdTe quantum is between 510nm-620nm.
7. when according to the method described in claim 1, it is characterised in that the spin speed of spin coating instrument is 1000rpm-2500rpm,
Between be 30s-60s.
8. according to the method described in claim 1, it is characterised in that described hydrophobic substrate is one in glass, silicon chip or plastics
Kind.
9. gluing method according to claim 1, it is characterised in that the contact angle of described hydrophobic substrate is 10 ° -25 °.
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| CN201710225398.2A CN107119327B (en) | 2017-04-07 | 2017-04-07 | Method for preparing large-area non-cracking colloidal photonic crystal film |
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| CN201710225398.2A CN107119327B (en) | 2017-04-07 | 2017-04-07 | Method for preparing large-area non-cracking colloidal photonic crystal film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108099433A (en) * | 2017-12-19 | 2018-06-01 | 苏州中科纳福材料科技有限公司 | The preparation method of counter opal structure anti-counterfeiting transfer printing film |
| CN110042673A (en) * | 2019-04-28 | 2019-07-23 | 浙江理工大学 | A kind of large area fast preparation method of textile substrate surface photon crystal structure color coating |
| CN110536798A (en) * | 2017-04-18 | 2019-12-03 | 韩国铸造、安全印刷与Id卡操作公司 | Crystal film with photon and its manufacturing method, the anti-fake product comprising the crystal film with photon |
| CN111826995A (en) * | 2020-01-20 | 2020-10-27 | 北京印刷学院 | Preparation method of high-brightness narrow-band-gap high-adhesion structural color film |
| CN111929991A (en) * | 2020-08-10 | 2020-11-13 | 大连理工大学 | Method for rapidly preparing colloidal photonic crystal array chip by utilizing laser direct writing |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110536798A (en) * | 2017-04-18 | 2019-12-03 | 韩国铸造、安全印刷与Id卡操作公司 | Crystal film with photon and its manufacturing method, the anti-fake product comprising the crystal film with photon |
| JP2020522583A (en) * | 2017-04-18 | 2020-07-30 | コリア ミンティング, セキュリティ プリンティング アンド アイディー カード オペレーティング コーポレーションKorea Minting, Security Printing & Id Card Operating Corp. | Photonic crystal film, method for producing the same, and anti-counterfeit article including the same |
| JP7007400B2 (en) | 2017-04-18 | 2022-01-24 | コリア ミンティング，セキュリティ プリンティング アンド アイディー カード オペレーティング コーポレーション | Photonic crystal film, its manufacturing method and anti-counterfeiting articles containing it |
| US11541680B2 (en) | 2017-04-18 | 2023-01-03 | Korea Minting, Security Printing & Id Card Operating Corp. | Photonic crystal film, method for manufacturing same, and anti-forgery article comprising same |
| CN108099433A (en) * | 2017-12-19 | 2018-06-01 | 苏州中科纳福材料科技有限公司 | The preparation method of counter opal structure anti-counterfeiting transfer printing film |
| CN110042673A (en) * | 2019-04-28 | 2019-07-23 | 浙江理工大学 | A kind of large area fast preparation method of textile substrate surface photon crystal structure color coating |
| CN110042673B (en) * | 2019-04-28 | 2022-06-17 | 浙江理工大学 | Large-area rapid preparation method of photonic crystal structure color coating on surface of textile substrate |
| CN111826995A (en) * | 2020-01-20 | 2020-10-27 | 北京印刷学院 | Preparation method of high-brightness narrow-band-gap high-adhesion structural color film |
| CN111929991A (en) * | 2020-08-10 | 2020-11-13 | 大连理工大学 | Method for rapidly preparing colloidal photonic crystal array chip by utilizing laser direct writing |
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