CN104409660A - Polymer-based white light OLED and preparation method thereof - Google Patents
Polymer-based white light OLED and preparation method thereof Download PDFInfo
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- CN104409660A CN104409660A CN201410626263.3A CN201410626263A CN104409660A CN 104409660 A CN104409660 A CN 104409660A CN 201410626263 A CN201410626263 A CN 201410626263A CN 104409660 A CN104409660 A CN 104409660A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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- H10K85/341—Transition metal complexes, e.g. Ru(II)polypyridine complexes
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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Abstract
The invention discloses a polymer-based white light OLED and a preparation method thereof. The polymer-based white light OLED comprises an ITO glass base layer, a hole transporting layer, a light emitting layer, an electron transporting layer and a metal cathode layer from the bottom up, wherein the ITO glass base layer takes ITO conductive glass as a substrate and an anode of the device, PEDOT:PSS acts as a hole injection layer and an electrode modification layer so as to further forms the hole transporting layer, TPBI is the electron transporting layer of the device, and calcium and silver form the metal cathode layer. The polymer-based white light OLED is characterized in that the light emitting layer is formed by subject materials PVK and OXD-7 and object materials FIrpic and Ir(bt)2(acac). The device provided by the invention can keep very stable spectrum emission when the brightness is within a range of 100cd m<-2> to 20000cd m<-2>, and a problem that polymer complementary-color white light OLED devices are unstable in spectrum is solved, thereby being conducive to realizing practical application of devices of the type.
Description
Technical field
The present invention relates to Organic Light Emitting Diode field, refer more particularly to a kind of Polymers white light OLED and preparation method thereof.
Background technology
OLED (Organic Light Emitting Diodes, Organic Light Emitting Diode) is because himself is frivolous, and the advantages such as self-luminous, have broad application prospects in display and solid-state illumination field.White light OLED device generally can be divided into complementary colours white light parts, three primary colors white light parts and four primary white light parts four class, wherein complementary colours device especially polymer body complementary colours phosphorescence white light OLED device due to composition simple, energy conversion efficiency is high, and there is the low energy consumption of solution processing method, easy and simple to handle, be beneficial to the advantages such as large-scale production, obtain at white light OLED lighting field and study widely.
A class PVK (Poly (N-vinylcarbazole) has prepared in Cao seminar in 2008, poly-(N-vinylcarbazole)) the high efficiency individual layer phosphorescence white light OLED device of main body, maximum external quantum efficiency reaches 12.9%, but the spectrum of device is very unstable, with the increase of current density, the relative intensity of blue light components presents the trend (Cao.Y first increasing and reduce, Wu.H.B, Adv.Mater.2008,20,696).2011, this seminar reports out another kind of efficient PVK main body individual layer complementary colours phosphorescence white light OLED device, and explore the reason that this base polymer phosphorescence white light parts spectrum changes with voltage, report points out that the unsteadiness of device spectral is (Wu.H.B caused by competition owing to occurring in luminescent layer under electric field action between hole capture on the narrower object of band gap and interference-free hole transport, Wong.W.Y, Cao.Y, Adv.Mater.2011,23,2976).But, until now, still can there is certain skew along with change in voltage in the polymer body complementary colours phosphorescence white light OLED device spectral reported out, spectrum instability problem is not still resolved (Ying.L, Wu.H.B, Wong.W.Y, Adv.Mater.2014,26,2459).
Summary of the invention
For solving the problems of the technologies described above, the technical solution adopted in the present invention is as follows:
A kind of Polymers white light OLED device, is respectively ito glass basalis, hole transmission layer, luminescent layer, electron transfer layer, metal cathode layer from down to up; Ito glass basalis is substrate using ITO electro-conductive glass as device and anode, PEDOT:PSS forms hole transmission layer further as hole injection layer and electrode modification layer, TPBI is the electron transfer layer of device, calcium and silver form metal cathode layer, it is characterized in that luminescent layer is by material of main part PVK and OXD-7, guest materials FIrpic, Ir (bt)
2(acac) form.
The electron transfer layer of above-mentioned Polymers white light OLED device, luminescent layer, TPBI, calcium, silver-colored thickness are respectively 35 nanometers, 55 nanometers, 35 nanometers, 10 nanometers, 100 nanometers.
The above-mentioned material of main part of Polymers white light OLED device and the ratio of guest materials are PVK:OXD-7:FIrpic:Ir (bt)
2(acac)=7:3:1:(0.03-0.04).
A preparation method for Polymers white light OLED device, comprises the steps:
Step one: ITO electro-conductive glass as the substrate of device and anode, after cutting and etching, successively through washing agent cleaning, ultra-pure water, acetone, ethanol three step ultrasonic cleaning process drying.
Step 2: by the ito glass of oven dry in step one through UV ozone process 15 minutes.
Step 3: on the ito glass handled well in step 2, spin coating PEDOT:PSS stoste is as hole injection layer, and the effect playing the substrate of lubrication ito glass.
Step 4: the substrate that spin coating in step 3 is good is put into after air dry oven is annealed 20 minutes at 120 DEG C and transfer to nitrogen glove box.
Step 5: sufficient for the dissolving prepared in advance luminescent layer mixed solution is spun on step 4 and has moved back on the substrate of fire, the thermal station that is placed on anneal 20 minutes at 120 DEG C.
Step 6: the substrate in step 5 is then transferred in multi-source organic molecule vacuum evaporation system, is evacuated to chamber pressure lower than 9 × 10
-5after Pa, the maintenance TPBI that then evaporation one deck 35nm is thick is at this pressure as electron transfer layer, after stopping heating, under this vacuum state, source temperature to be evaporated is cooled to less than 60 DEG C, and substrate therefrom takes out by the nitrogen be filled with in glove box to evaporation chamber to normal pressure.
Step 7: the substrate of step 6 is then put into multi-source metal vacuum deposition system, be evacuated to chamber pressure lower than 9 × 10
-5after Pa, the calcium that evaporation one deck 10nm is thick successively and the silver of one deck 100nm are as metallic cathode.
Step 8: plated film terminates, treats under keeping this vacuum state that cooling of electrode is to room temperature, is then filled with nitrogen in glove box to normal pressure to chamber, takes out substrate, namely obtains single-shot photosphere Polymers white light OLED device prepared by solwution method.
In described step one, to ITO substrate washing agent clean, require that the surface after process does not have macroscopic stain, impurity under light illumination.
In described step one, the step of ultra-pure water, acetone, the ultrasonic cleaning of ethanol three step, its ultrasonic time is followed successively by 10 minutes, 20 minutes, 20 minutes.
In described step 2, the operating power of the UV ozone cleaning machine adopted is 100W.
In described step 3, need first through the filtration of water-based filter before spin coating PEDOT:PSS stoste, filter specification is 0.25 μm.
In described step 3, the spincoating conditions parameter of PEDOT:PSS stoste is rotating speed 1500rps (rev/min), and the time sets 50 seconds.
In described step 5, the solution concentration prepared is 16mg/mL.Spincoating conditions parameter is rotating speed 3000rps, and the time sets 30 seconds.
In described step 6, the evaporation rate of TPBI is
in step 7, the evaporation rate of calcium metal is
the evaporation rate of argent is
the speed of growth and the thickness of film are monitored by film thickness gauge.
The operation of described step one to four is carried out all in atmosphere.
The operation of described step 5 to eight is all carried out in vacuum glove box, and glove box atmosphere controls at water content <1ppm, oxygen content <1ppm.
Advantage of the present invention:
1, device provided by the present invention is 100-20000cd m in brightness
-2scope in all can keep very stable spectral emissions, successfully solve the problem of polymer complementary colours white light OLED device spectral instability, be conducive to such device and realize application in practice.
2, while device provided by the invention has excellent spectrum property, be 1000cd m in brightness
-2time luminous efficiency also up to 25.5cd A
-1, reach the level suitable with conventional incandescent lamp, have broad application prospects at OLED solid-state white lighting field.
3, device provided by the present invention adopts the preparation of solution processing method, and easy and simple to handle, with low cost, energy savings, is conducive to large-scale batch production.
4, the spin coating annealing of method luminescent layer provided by the invention and preparation process afterwards all complete in glove box, avoid the erosion that the water oxygen in air causes device, the organic solvent simultaneously adopted is common low poison solvent, reduce the pollution to environment and harm, preparation process environmental protection.
Accompanying drawing explanation
Fig. 1 organic electroluminescence device structure chart of the present invention.
The electroluminescent spectrum of the complementary colours white light parts that Fig. 2 adopts the present invention to prepare.
The spectrogram that the device that Fig. 3 adopts the present invention to prepare changes with brightness.
Device current density vs. voltage-luminosity response that Fig. 4 adopts the present invention to prepare.
Device luminous efficiency-brightness-power efficiency characteristic curve that Fig. 5 adopts the present invention to prepare.
Embodiment
Implementation method of the present invention is set forth below in conjunction with specific embodiment.
The warm white device architecture that the present invention relates to as shown in Figure 1, wherein ITO (Indium Tin Oxides, tin indium oxide) electro-conductive glass is as the substrate of device and anode, PEDOT:PSS (the Poly-(3 that one deck 35nm is thick, 4-ethylenedioxythiophene) Polystyrene sulfonate, poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid)) as hole injection layer and electrode modification layer.Luminescent layer by material of main part by PVK and OXD-7 (2,2'-(1,3-Phenylene) bis [5-(4-tert-butylphenyl)-1,3,4 – oxadiazole], 2,2'-(1,3-phenyl) two [5-(4-tert-butyl-phenyl)-1,3,4-oxadiazoles]), guest materials FIrpic (Bis (4,6-difluorophenyl-pyridinato-N, C2) picolinatoiridium, two (4,6-difluorophenyl pyridinato-N, C2) pyridinecarboxylic close iridium), Ir (bt)
2(acac) (Bis (2-phenyl-benzothiazole-C2, N) (acetylacet-onate) iridium (III), acetopyruvic acid two (2-phenylbenzothiazol-C2, N) iridium (III) is closed) blended doping in certain proportion obtains, and luminescent layer gross thickness is 55nm.The TPBI (1 that above luminescent layer, evaporation one deck 35nm is thick, 3,5-Tri (1-phenyl-1H-benzo-[d] imidazol-2-yl) phenyl, 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene) be the electron transfer layer of device, then above successively the calcium of evaporation one deck 10nm and the silver of 100nm as metal electrode.The light-emitting area of final obtained device is 6mm
2.
In order to prepare above-mentioned warm white device, in concrete enforcement, the ito glass used by the present invention is bought in Shenzhen Nanbo Display Device Science & Technology Co., Ltd., and PEDOT:-PSS is purchased from Bayer A.G, PVK, OXD-7, FIrpic, Ir (bt)
2(acac) all buy in Aldrich chemical reagents corporation.
When prepared by reality, in laboratory, room temperature remains at 21 DEG C, and humidity is always less than 35%.
Concrete preparation method is as follows:
Step one: first the ito glass substrate after cutting and etching is cleaned with washing agent, the impurity on removing surface and greasy dirt, then successively through ultra-pure water ultrasonic cleaning 10 minutes, acetone ultrasonic cleaning 20 minutes, EtOH Sonicate cleans three step ultrasonic cleaning process in 20 minutes and is placed on oven for drying.
Step 2: a kind of for above-mentioned steps ito glass substrate of oven dry being placed in power is that the UV ozone processing instrument of 100W carries out UV ozone process 15 minutes.
Step 3: on the substrate handled well in step 2 and then spin coating one deck PEDOT:PSS as hole injection layer.The water-based filtering head adding 0.25 μm during spin coating filters PEDOT:PSS stoste, and the rotating speed spin coating of employing 1500rps 50 seconds, obtains the uniformly transparent film of one deck 35nm.
Step 4: the substrate in above-mentioned steps three is put into the nitrogen glove box transferred to water oxygen content after air dry oven is annealed 20 minutes at 120 DEG C and be all less than 1ppm.
Step 5: the sufficient luminescent layer mixed solution of dissolving is spun on the above-mentioned substrate having moved back fire with the rotating speed of 3000rps, set of time 30 seconds.Film forming is placed on thermal station and anneals 20 minutes at 120 DEG C.Luminescent solution adopts chlorobenzene as solvent, and concentration is 16mg/mL, and concrete composition is (PVK:OXD-7:FIrpic (7:3:1)): 0.3%-0.4%Ir (bt)
2(acac), its ratio used is mass ratio.。
Step 6: and then substrate above-mentioned steps five having been moved back fire is transferred in multi-source organic molecule vacuum evaporation system, is evacuated to chamber pressure lower than 9 × 10
-5after Pa, keep at this pressure then with
the thick TPBI of speed evaporation one deck 35nm as electron transfer layer, after stopping heating, under this vacuum state, source temperature to be evaporated is cooled to less than 60 DEG C, is filled with nitrogen in glove box to normal pressure, is taken out by substrate to evaporation chamber.
Step 7: then the substrate of above-mentioned steps six is put into multi-source metal vacuum deposition system, be evacuated to chamber pressure lower than 9 × 10
-5after Pa, successively respectively with
with
the thick calcium of speed evaporation one deck 10nm and the silver of one deck 100nm as metallic cathode.
Step 8: after plated film terminates, treats under keeping this vacuum state that cooling of electrode is to room temperature, is then filled with nitrogen in glove box to normal pressure to chamber, takes out substrate, obtains single-shot photosphere Polymers white light OLED device prepared by solution processing method.
Wherein water miscible PEDOT:PSS is a kind of conventional ITO interface-modifying layer, is usually spun on and cleans up and on the ITO layer of ultraviolet irradiation process, form the film of one deck flat transparent, as hole injection layer.TPBI is a kind of conventional electron transport layer materials, and in the present invention, for the consideration of level-density parameter and carrier transport balance aspect, electron transport material selects TPBI.OXD-7 is a kind of common electron transport material, itself and material of main part is carried out doping and forms hybrid agent, can increase the electric conductivity of material of main part, improves device light emitting efficiency.FIrpic, Ir (bt)
2(acac) be common two kinds of phosphorescent colorings, be used separately as blue light object and orange red smooth object.
Chlorobenzene has good dissolubility for most of organic substance, and chlorobenzene solution has excellent filming performance, and in the present invention, the preparation of luminescent layer solution adopts chlorobenzene as solvent.
Fig. 2 gives the electroluminescent spectrum of device.CIE (the Commission International deL ' Eclairage of obtained device, Commission Internationale De L'Eclairage) chromaticity coordinates is (0.365,0.426), drop in white light field, CCT (CorrelatedColour Temperature, correlated colour temperature) is 4650K, belongs to low color temperature light sources category, CRI (Color Rendering Index, color rendering index) is up to 72.Excellent look quality parameter proves that Polymers complementary colours white light OLED device provided by the present invention is a kind of solid-state lighting device of great potential.
Fig. 3 gives the employing spectrogram that polymer complementary colours white light parts prepared by the present invention changes with brightness.At brightness 100-20000cd m
-2scope in the electroluminescent spectrum curve of device almost present the consistency of height, demonstrate the spectrum stability that device is good.
Fig. 4 gives the Current density-voltage-luminosity response of polymer complementary colours white light parts provided by the present invention.Can find out, the bright voltage that opens of device is 4.8V, and maximum current density is close to 500mA cm
-2, high-high brightness can reach 50000cd m
-2.
As shown in Figure 5, device is 4630cd m in brightness to the luminous efficiency-brightness-power efficiency characteristic curve of device
-2time reach 25.5cd A
-1maximum lumen efficiency, be 1000cd m in current density
-2time, lumen is still up to 19.5cd A
-1, suitable with conventional incandescent lamp efficiency.Good Devices Electroluminescent performance, gives the credit to the use of high performance material and the optimal design to this body structure of device.
All test results show, Polymers complementary colours white light parts function admirable involved in the present invention, chromaticity matter is high, and spectrum stability is good, and preparation process is easy and simple to handle, with low cost, energy savings, and is beneficial to large-scale production.The research and development of the present invention to high chromaticity matter high-performance complementary look white light OLED has important impetus, and has huge commercial application potentiality at solid-state white lighting field from now on.
Claims (10)
1. a Polymers white light OLED device, is respectively ito glass basalis, hole transmission layer, luminescent layer, electron transfer layer, metal cathode layer from down to up; Ito glass basalis is substrate using ITO electro-conductive glass as device and anode,
PEDOT:PSS forms hole transmission layer further as hole injection layer and electrode modification layer, TPBI is the electron transfer layer of device, calcium and silver form metal cathode layer, it is characterized in that luminescent layer is by material of main part PVK and OXD-7, guest materials FIrpic, Ir (bt)
2(acac) form.
2. a kind of Polymers white light OLED device according to claim 1, it is characterized in that electron transfer layer, luminescent layer, TPBI, calcium, silver thickness be respectively 35 nanometers, 55 nanometers, 35 nanometers, 10 nanometers, 100 nanometers.
3. a kind of Polymers white light OLED device according to claim 1, is characterized in that the ratio of material of main part and guest materials is PVK:OXD-7:FIrpic:Ir (bt)
2(acac)=7:3:1:(0.03-0.04).
4. a preparation method for Polymers white light OLED device, comprises the steps:
Step one: ITO electro-conductive glass as the substrate of device and anode, after cutting and etching, successively through washing agent cleaning, ultra-pure water, acetone, ethanol three step ultrasonic cleaning process drying;
Step 2: by the ito glass of oven dry in step one through UV ozone process 15 minutes;
Step 3: on the ito glass handled well in step 2, spin coating PEDOT:PSS stoste is as hole injection layer, and the effect playing the substrate of lubrication ito glass;
Step 4: the substrate that spin coating in step 3 is good is put into after air dry oven is annealed 20 minutes at 120 DEG C and transfer to nitrogen glove box;
Step 5: sufficient for the dissolving prepared in advance luminescent layer mixed solution is spun on step 4 and has moved back on the substrate of fire, the thermal station that is placed on anneal 20 minutes at 120 DEG C;
Step 6: the substrate in step 5 is then transferred in multi-source organic molecule vacuum evaporation system, is evacuated to chamber pressure lower than 9 × 10
-5after Pa, the maintenance TPBI that then evaporation one deck 35nm is thick is at this pressure as electron transfer layer, after stopping heating, under this vacuum state, source temperature to be evaporated is cooled to less than 60 DEG C, and substrate therefrom takes out by the nitrogen be filled with in glove box to evaporation chamber to normal pressure;
Step 7: the substrate of step 6 is then put into multi-source metal vacuum deposition system, be evacuated to chamber pressure lower than 9 × 10
-5after Pa, the calcium that evaporation one deck 10nm is thick successively and the silver of one deck 100nm are as metallic cathode;
Step 8: plated film terminates, treats under keeping this vacuum state that cooling of electrode is to room temperature, is then filled with nitrogen in glove box to normal pressure to chamber, takes out substrate, namely obtains single-shot photosphere Polymers white light OLED device prepared by solwution method.
5. the preparation method of a kind of Polymers white light OLED device according to claim 4, it is characterized in that the step of described step one ultra-pure water, acetone, the ultrasonic cleaning of ethanol three step, its ultrasonic time is followed successively by 10 minutes, 20 minutes, 20 minutes.
6. the preparation method of a kind of Polymers white light OLED device according to claim 4, it is characterized in that in described step 3, need first through the filtration of water-based filter before spin coating PEDOT:PSS stoste, filter specification is 0.25 μm.
7. the preparation method of a kind of Polymers white light OLED device according to claim 4, is characterized in that in described step 3, and the spincoating conditions parameter of PEDOT:PSS stoste is rotating speed 1500rps (rev/min), and the time sets 50 seconds.
8. the preparation method of a kind of Polymers white light OLED device according to claim 4, it is characterized in that in described step 5, the solution concentration prepared is 16mg/mL; Spincoating conditions parameter is rotating speed 3000rps, and the time sets 30 seconds.
9. the preparation method of a kind of Polymers white light OLED device according to claim 4, it is characterized in that in described step 6, the evaporation rate of TPBI is
in step 7, the evaporation rate of calcium metal is
the evaporation rate of argent is
the speed of growth and the thickness of film are monitored by film thickness gauge.
10. the preparation method of a kind of Polymers white light OLED device according to claim 4, is characterized in that the operation of described step one to four is carried out all in atmosphere; The operation of described step 5 to eight is all carried out in vacuum glove box, and glove box atmosphere controls at water content <1ppm, oxygen content <1ppm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105374945A (en) * | 2015-11-27 | 2016-03-02 | 南京邮电大学 | Organic white light device and preparation method thereof |
| CN105938876A (en) * | 2016-05-11 | 2016-09-14 | 南京邮电大学 | Environment-friendly organic electroluminescence device and preparation method thereof |
| CN107359179A (en) * | 2017-07-07 | 2017-11-17 | 安徽熙泰智能科技有限公司 | A kind of preparation method of OLED micro-display devices |
| CN114038947A (en) * | 2020-11-03 | 2022-02-11 | 广东聚华印刷显示技术有限公司 | Method for processing functional layer of light-emitting device and light-emitting device |
| CN114038947B (en) * | 2020-11-03 | 2024-05-17 | 广东聚华印刷显示技术有限公司 | Method for processing functional layer of light-emitting device and light-emitting device |
-
2014
- 2014-11-07 CN CN201410626263.3A patent/CN104409660A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105374945A (en) * | 2015-11-27 | 2016-03-02 | 南京邮电大学 | Organic white light device and preparation method thereof |
| CN105938876A (en) * | 2016-05-11 | 2016-09-14 | 南京邮电大学 | Environment-friendly organic electroluminescence device and preparation method thereof |
| CN107359179A (en) * | 2017-07-07 | 2017-11-17 | 安徽熙泰智能科技有限公司 | A kind of preparation method of OLED micro-display devices |
| CN114038947A (en) * | 2020-11-03 | 2022-02-11 | 广东聚华印刷显示技术有限公司 | Method for processing functional layer of light-emitting device and light-emitting device |
| CN114038947B (en) * | 2020-11-03 | 2024-05-17 | 广东聚华印刷显示技术有限公司 | Method for processing functional layer of light-emitting device and light-emitting device |
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