CN103151450A - Ultraviolet-enhanced composite film based on quantum point and preparation method thereof - Google Patents
Ultraviolet-enhanced composite film based on quantum point and preparation method thereof Download PDFInfo
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- CN103151450A CN103151450A CN2013100665388A CN201310066538A CN103151450A CN 103151450 A CN103151450 A CN 103151450A CN 2013100665388 A CN2013100665388 A CN 2013100665388A CN 201310066538 A CN201310066538 A CN 201310066538A CN 103151450 A CN103151450 A CN 103151450A
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Abstract
The invention discloses an ultraviolet-enhanced composite film based on a quantum point and a preparation method thereof. The ultraviolet-enhanced composite film based on the quantum point comprises a bottom layer quartz substrate, a poly-3,4-ethylenedioxy thiophene/polystyrene sulfonate film layer, poly-4-butyl triphenylamine film layer and a quantum point film layer from bottom to top in sequence; the poly-3,4-ethylenedioxy thiophene/polystyrene sulfonate film layer, the poly-4-butyl triphenylamine film layer and the quantum point film layer are formed by coating films through a spin coating method or a czochralski method. As the ultraviolet-enhanced composite film provided by the invention contains the poly-3,4-ethylenedioxy thiophene/polystyrene sulfonate film layer and the poly-4-butyl triphenylamine film layer, light scattering on the ultraviolet-enhanced single-layered film surface is reduced, the light emitting capability of the ultraviolet-enhanced single-layered film is enhanced, particularly the light emitting efficiency of the deep ultraviolet wave band is enhanced, thereby providing effective means for the application of the quantum point in the ultraviolet-enhanced film.
Description
Technical field
The present invention relates to a kind of compound ultraviolet enhanced film based on quantum dot and preparation method thereof.
Background technology
The quantum dot fluorescence life-span is long, have wide excitation spectrum and narrow emission spectra, emission wavelength to be subjected to the advantage such as quantum dot size control to be widely used in the numerous areas such as LED, biological detection.And for silica-based image device, due to itself for the ultraviolet band response ratio a little less than, institute thinks that strengthening its ultraviolet responds, begin both at home and abroad extensively ultraviolet frequency conversion film to be studied, the organic frequency conversion film of original main employing and inorganic frequency conversion film bi-material, organic frequency conversion membrane technology is relatively ripe, also has relevant patent to occur., but such film has fatal shortcoming, and it is very fast that is exactly organic molecule degradation speed under ultra-violet radiation.Be 1 μ W/cm in illuminance
2Illumination under, organic molecule is with up to per hour 3% speed exponentially degraded.So carry out the research for inorganic frequency conversion film.Inorganic fluorescent material normally is comprised of rare earth oxide and catalyst, and the crystal diameter of inorganic fluorescent material is generally at 1-150 μ m.Therefore, although the thin-film light emitting time (life-span) that the method that precipitates with spin coating prepares is quite long, generally can reach 5500h, also there are many defectives in the film gauge uniformity of preparation etc.
Quantum dot film is a kind of emerging material, yet quantum dot film mainly is based on the individual layer ultraviolet enhanced film of quantum dot at present, and should be very low at ultraviolet band especially deep ultraviolet wave band luminous efficiency based on the individual layer ultraviolet enhanced film of quantum dot.Strengthen if can be applied to ultraviolet, just native defect can be solved, and make its conversion efficiency obviously strengthen.
Summary of the invention
One of purpose of the present invention is to provide a kind of compound ultraviolet enhanced film based on quantum dot in order to solve the above-mentioned individual layer ultraviolet enhanced film based on quantum dot in the ultraviolet band technical problem that especially deep ultraviolet wave band luminous efficiency is very low.
Two of purpose of the present invention is to provide the preparation method of above-mentioned a kind of compound ultraviolet enhanced film based on quantum dot.
Technical scheme of the present invention
A kind of compound ultraviolet enhanced film based on quantum dot, be layer structure, comprise quartz substrate, quantum dot film layer, also comprise poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer and poly-4-butyl triphenylamine thin layer, be followed successively by the quantum dot film layer of bottom quartz substrate, poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer, poly-4-butyl triphenylamine thin layer and the superiors from bottom to top;
Described quantum dot film layer is CdSe/ZnS nuclear shell structure quantum point thin layer;
Described poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer and poly-4-butyl triphenylamine thin layer and quantum dot film layer form by spin-coating method plated film or czochralski method plated film.
The preparation method of above-mentioned a kind of compound ultraviolet enhanced film based on quantum dot specifically comprises the steps:
(1), quartz substrate is cleaned through deionized water, propyl alcohol, ethanol, b propanol successively, then it is clean to pass through ultrasonic cleaning
(2), will gather 3, on quartz substrate after the polystyrolsulfon acid solution of 4-Ethylenedioxy Thiophene/polystyrolsulfon acid cleans to step (1) by rotary process plated film or czochralski method plated film, putting into baking oven after plated film toasts, temperature is 150 ℃, after time is 30min, obtain poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer;
Described poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid solution is that solid content is 1% poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid solution;
(3), will gather again 4-butyl triphenylamine solution and arrive poly-3 by rotation plating method film or czochralski method plated film, on 4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer, put into baking oven after plated film and toast, temperature is 120 ℃, and the time is to obtain poly-4-butyl triphenylamine thin layer after 30min;
Described poly-4-butyl triphenylamine solution is poly-4-butyl triphenylamine to be dissolved in chlorobenzene reagent form, and the poly-4-butyl triphenylamine that concrete proportioning is 10mg is to be dissolved in chlorobenzene 1ml reagent;
(4), again with quantum dot solution by rotary process plated film or czochralski method plated film to poly-4-butyl triphenylamine thin layer, putting into baking oven after plated film toasts, toast 80 ℃, obtain the quantum dot film layer after 20min, finally obtain the compound ultraviolet enhanced film based on quantum dot;
Described quantum dot solution is the CdSe/ZnS nuclear shell structure quantum point to be dissolved in toluene solvant form, and the CdSe/ZnS nuclear shell structure quantum point that concrete proportioning is 5mg is dissolved in 1ml toluene, and the particle diameter of CdSe/ZnS nuclear shell structure quantum point is preferably 5nm.
A kind of compound ultraviolet enhanced film based on quantum dot of above-mentioned gained is applied to silica-based image device ultraviolet and strengthens use.
Beneficial effect of the present invention
a kind of compound ultraviolet enhanced film based on quantum dot of the present invention, owing to containing poly-3, 4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer and poly-4-butyl triphenylamine thin layer, thereby reduced the scattering of light based on the compound ultraviolet enhanced film surface of quantum dot, and then strengthened its luminous power, particularly deep ultraviolet wave band luminous efficiency is enhanced, so a kind of compound ultraviolet enhanced film based on quantum dot of the present invention, having solved original individual layer ultraviolet enhanced film based on quantum dot has especially solved in the lower problem of dark purple place wave band (190nm) luminous efficiency in the lower problem of ultraviolet band luminous efficiency, effective means are provided for quantum dot in the application of ultraviolet enhanced film.
Further, a kind of roughness test of compound ultraviolet enhanced film under the AFM atomic force microscope based on quantum dot of the present invention, final result show that the roughness of film surface reduces, and then reduce scattering of light, have effectively improved luminous efficiency.
Description of drawings
The structural representation based on the compound ultraviolet enhanced film of quantum dot in Fig. 1, embodiment 1, wherein 1 is that quartz substrate, 2 is the quantum dot film layer for gathering 3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer, 3 for gathering 4-butyl triphenylamine thin layer and 4;
The structural representation based on the individual layer ultraviolet enhanced film of quantum dot in Fig. 2, comparative examples, wherein 1 is that quartz substrate, 2 is the quantum dot film layer;
Fig. 3,190nm deep ultraviolet excite compound ultraviolet enhanced film based on quantum dot, based on the luminescent spectrum of the individual layer ultraviolet enhanced film of quantum dot.
Embodiment
Also by reference to the accompanying drawings the present invention is further set forth below by specific embodiment, but do not limit the present invention.
The 650-23NPP spin coating instrument that the equipment that in various embodiments of the present invention, rotary plating uses is produced as Mycro Technologies; Ultrasonic cleaning equipment used is the KQ5200DE type numerical control supersonic cleaning apparatus that Kunshan Ultrasonic Instruments Co., Ltd. produces.
In various embodiments of the present invention, solvent chlorobenzene, toluene used is and analyzes alcohol, and Shanghai Ling Feng chemical reagent Co., Ltd produces.
A kind of compound ultraviolet enhanced film based on quantum dot, be layer structure, its structural representation is followed successively by quartz substrate 1, poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer 2, poly-4-butyl triphenylamine thin layer 3 and the quantum dot film layer 4 of bottom from bottom to top as shown in Figure 2;
Described quantum dot film layer 4 is CdSe/ZnS nuclear shell structure quantum point thin layer;
Described poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer 2 and poly-4-butyl triphenylamine thin layer 3 and quantum dot film layer 4 are to form by the spin-coating method plated film.
The preparation method of above-mentioned a kind of compound ultraviolet enhanced film based on quantum dot specifically comprises the steps:
(1), quartz substrate 1 is cleaned through deionized water, propyl alcohol, ethanol, b propanol successively, then it is clean to pass through ultrasonic cleaning;
(2), will gather 3, on quartz substrate after 4-Ethylenedioxy Thiophene/polystyrolsulfon acid solution cleans to step (1) by rotary process plated film plated film, rotating speed is 1500r/min, putting into baking oven after plated film toasts, temperature is 150 ℃, time obtains poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer after being 30min;
Described poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid solution is that solid content is 1% poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid solution;
(3), will gather again 4-butyl triphenylamine solution by rotation plating method film plated film poly-3, on 4-Ethylenedioxy Thiophene/polystyrolsulfon acid layer, rotating speed is 1200r/min, puts into baking oven after plated film and toasts, temperature is 120 ℃, and the time is to obtain poly-4-butyl triphenylamine thin layer after 30min;
Described poly-4-butyl triphenylamine solution is poly-4-butyl triphenylamine to be dissolved in chlorobenzene reagent form, and the poly-4-butyl triphenylamine that concrete proportioning is 10mg is to be dissolved in chlorobenzene 1ml reagent;
(4), again with quantum dot solution by the rotary process plated film to poly-4-butyl triphenylamine thin layer, rotating speed is 1000r/min, puts into baking oven after plated film and toasts, and toasts 80 ℃, obtain the quantum dot film layer after 20min, finally obtain the compound ultraviolet enhanced film based on quantum dot;
Described quantum dot solution is the CdSe/ZnS nuclear shell structure quantum point that particle diameter is 5nm to be dissolved in toluene solvant form, and the CdSe/ZnS nuclear shell structure quantum point that concrete proportioning is 5mg is dissolved in 1ml toluene.
Comparative examples
A kind of individual layer ultraviolet enhanced film based on quantum dot is the layer structure of 2 layers, and its structural representation comprises the quartz substrate 1 of bottom and the quantum dot film layer 2 on upper strata as shown in Figure 2;
Described quantum dot film layer 2 is CdSe/ZnS nuclear shell structure quantum point thin layer;
Described quantum dot film layer forms by the spin-coating method plated film.
The preparation method of above-mentioned a kind of individual layer ultraviolet enhanced film based on quantum dot specifically comprises the steps:
(1), quartz substrate 1 is cleaned through deionized water, propyl alcohol, ethanol, b propanol successively after, then it is clean to pass through ultrasonic cleaning;
(2), with the surface of quanta point material rotary process plated film to quartz substrate 1, rotating speed is 1000r/min, puts into baking oven after plated film and toasts, 80 ℃ of bakings obtain the quantum dot film layer after 20min, namely get the individual layer ultraviolet enhanced film based on quantum dot;
It is that the CdSe/ZnS nuclear shell structure quantum point of 5nm is dissolved in and namely gets quanta point material in toluene solvant that described quanta point material is about to particle diameter, and the CdSe/ZnS nuclear shell structure quantum point that concrete proportioning is 5mg is dissolved in 1ml toluene.
the individual layer ultraviolet enhanced film based on quantum dot based on the compound ultraviolet enhanced film of quantum dot and comparative examples gained of above-described embodiment 1 gained is tested at the Chinese light ZLX-PL-1 fluorescence spectrum test macro of standing upright respectively and obtained measuring its luminescent spectrum under 190nm deep ultraviolet shooting condition, result as shown in Figure 3, composite quantum dot film in figure is the luminescent spectrum based on the compound ultraviolet enhanced film of quantum dot of gained in embodiment 1, individual layer quantum dot film in figure is the luminescent spectrum based on the compound ultraviolet enhanced film of quantum dot of comparative examples gained, as can be seen from Figure 3, the peak wavelength of the emission spectrum of two kinds of ultraviolet enhanced film all is positioned at the 480nm left and right, but the compound ultraviolet enhanced film based on quantum dot of gained in embodiment 1, the intensity of its emission peak is 345099, and the emission peak intensity based on the individual layer ultraviolet enhanced film of quantum dot of comparative examples gained is 4011, as seen the luminous intensity based on the compound ultraviolet enhanced film of quantum dot significantly improves.
With above-described embodiment 1 gained based on the compound ultraviolet enhanced film of quantum dot and comparative examples gained test its r.m.s. roughness Rq and arithmetic average roughness Ra respectively under the XE-100 type atomic force microscope that PARK company produces based on the individual layer ultraviolet enhanced film of quantum dot, its test result sees the following form:
| Film type | Rq (nm) | Ra (nm) |
| Quantum dot individual layer ultraviolet enhanced film | 9.116 | 7.205 |
| The compound ultraviolet enhanced film of quantum dot | 5.209 | 4.251 |
As can be seen from the above table, based on the Rq of the compound ultraviolet enhanced film of quantum dot and Ra all lower than the individual layer ultraviolet enhanced film based on quantum dot, roughness just because of having reduced based on the individual layer ultraviolet enhancing of quantum dot just makes and has reduced scattering of light, the luminous efficiency of enhancing.
In sum, a kind of composite quantum dot ultraviolet enhanced film of the present invention, owing to having increased poly-3 in the middle of the quantum dot film layer of bottom quartz substrate and the superiors, 4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer and poly-4-butyl triphenylamine thin layer, thereby reduced the scattering of light based on the individual layer ultraviolet enhanced film surface of quantum dot, and then strengthened its luminous power, particularly deep ultraviolet wave band luminous efficiency is obviously strengthened, and is a kind of efficient compound ultraviolet enhanced film based on quantum dot.
Foregoing is the basic explanation under conceiving for the present invention only, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (3)
1. the compound ultraviolet enhanced film based on quantum dot, be layer structure, comprises quartz substrate, quantum dot film layer, characterized by further comprising by poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer and poly-4-butyl triphenylamine thin layer;
Described a kind of compound ultraviolet enhanced film based on quantum dot is followed successively by the quantum dot film layer of bottom quartz substrate, poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer, poly-4-butyl triphenylamine thin layer and the superiors from bottom to top;
Described quantum dot film layer is CdSe/ZnS nuclear shell structure quantum point thin layer;
Described poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer, poly-4-butyl triphenylamine thin layer and quantum dot film layer form by spin-coating method plated film or czochralski method plated film.
2. a kind of compound ultraviolet enhanced film based on quantum dot as claimed in claim 1, the particle diameter that it is characterized in that described CdSe/ZnS nuclear shell structure quantum point is 5nm.
3. the preparation method of a kind of compound ultraviolet enhanced film based on quantum dot as claimed in claim 1 or 2, is characterized in that specifically comprising the steps:
(1), quartz substrate is cleaned through deionized water, propyl alcohol, ethanol, b propanol successively, then it is clean to pass through ultrasonic cleaning;
(2), will gather 3, on quartz substrate after 4-Ethylenedioxy Thiophene/polystyrolsulfon acid solution cleans to step (1) by rotary process plated film or czochralski method plated film, putting into baking oven after plated film toasts, temperature is 150 ℃, time is to form poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer after 30min;
Described poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid solution is that solid content is 1% poly-3,4-Ethylenedioxy Thiophene/polystyrolsulfon acid solution;
(3), will gather again 4-butyl triphenylamine solution and arrive poly-3 by rotation plating method film or czochralski method plated film, on 4-Ethylenedioxy Thiophene/polystyrolsulfon acid thin layer, put into baking oven after plated film and toast, temperature is 120 ℃, and the time is to form poly-4-butyl triphenylamine thin layer after 30min;
Described poly-4-butyl triphenylamine solution is poly-4-butyl triphenylamine to be dissolved in chlorobenzene reagent form, and the poly-4-butyl triphenylamine that concrete proportioning is 10mg is to be dissolved in chlorobenzene 1ml reagent;
(4), again with quantum dot solution by rotary process plated film or czochralski method plated film to poly-4-butyl triphenylamine thin layer, putting into baking oven after plated film toasts, toast 80 ℃, form the quantum dot thin layer after 20min, finally obtain the compound ultraviolet enhanced film based on quantum dot;
Described quantum dot solution is about to the CdSe/ZnS nuclear shell structure quantum point and is dissolved in toluene solvant and forms, and the CdSe/ZnS nuclear shell structure quantum point that concrete proportioning is 5mg is dissolved in 1ml toluene.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102447070A (en) * | 2010-10-09 | 2012-05-09 | 中国计量学院 | Quantum-dot OLED (Organic Light Emitting Diode) light emitting device of photonic crystal structure |
| CN102473800A (en) * | 2009-07-07 | 2012-05-23 | 佛罗里达大学研究基金会公司 | Stable and all solution processable quantum dot light-emitting diodes |
| CN102723440A (en) * | 2012-06-26 | 2012-10-10 | 吉林大学 | ZnCuInS/ZnS quantum dot white light LED (Light Emitting Diode) based on compensation light emitting and manufacturing method thereof |
| CN203218326U (en) * | 2013-03-04 | 2013-09-25 | 上海理工大学 | Ultraviolet-enhanced composite film based on quantum point |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102473800A (en) * | 2009-07-07 | 2012-05-23 | 佛罗里达大学研究基金会公司 | Stable and all solution processable quantum dot light-emitting diodes |
| CN102447070A (en) * | 2010-10-09 | 2012-05-09 | 中国计量学院 | Quantum-dot OLED (Organic Light Emitting Diode) light emitting device of photonic crystal structure |
| CN102723440A (en) * | 2012-06-26 | 2012-10-10 | 吉林大学 | ZnCuInS/ZnS quantum dot white light LED (Light Emitting Diode) based on compensation light emitting and manufacturing method thereof |
| CN203218326U (en) * | 2013-03-04 | 2013-09-25 | 上海理工大学 | Ultraviolet-enhanced composite film based on quantum point |
Non-Patent Citations (1)
| Title |
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| 聂海，张波，唐先忠，李元勋: "聚TPD电荷传输材料的制备与单层器件的电致发光", 《北京科技大学学报》 * |
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Application publication date: 20130612 |