CN104409661A - Complementary-color phosphorescence white light OLED (organic light emitting diode) and preparation method thereof - Google Patents
Complementary-color phosphorescence white light OLED (organic light emitting diode) and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a complementary-color phosphorescence white light OLED (organic light emitting diode) and a preparation method thereof. The complementary-color phosphorescence 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 a device, PEDOT:PSS acts as a hole injection layer and an electrode modification layer so as to further form the hole transporting layer, TPBI acts as the electron transporting layer of the device, calcium and silver form the metal electrode layer, and the characteristic is that the light emitting layer is formed by subject materials DTPAFB and OXD-7 and object materials FIrpic and Ir(bt)2(acac). The CRI (color rendering index) of the complementary-color phosphorescence white light LED provided by the invention reaches up to 71, which is the highest level of the CRI of complementary-color white light OLED devices which take triphenylamine derivative small molecules as the subject materials, and the difference between such devices and an ideal white light illumination light source is greatly reduced.
Description
Technical field
The present invention relates to Organic Light Emitting Diode field, refer more particularly to a kind of complementary colours phosphorescence white light OLED device 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.OLED white-light illuminating device can be divided into complementary colours white light parts, three primary colors white light parts and four primary white light parts three kinds, wherein complementary colours device especially host-guest system complementary colours white light parts due to composition simple, be easy to realize and there is high luminous efficiency, obtain at white light OLED lighting field and study widely.
Triphenylamine micromolecular is owing to having higher triplet, and the many advantages such as good bipolarity and excellent film morphological stability, receive general concern in the small molecule host material research of phosphorescent OLED device.2012, the people such as Yang report the novel triphenylamine derivative bipolarity Small molecular TCTAPO of a class ((9-(4-(bis (4-(9H-carbazol-9-yl) phenyl) amino)-phenyl)-9H-carbazol-3-yl) diphenylphosphineoxide, (9-(4-(two (4-(9 hydrogen-carbazole-9-base) phenyl) amino)-phenyl)-9 hydrogen-carbazole-3-base) diphenylphosphine oxygen) be the complementary colours phosphorescence white light parts of material of main part, obtain 47.0lm W
-1high efficiency, but the CRI of device is (Color Rendering Index, color rendering index) but lower than 60, need reach for the requirement of 80 relative to desirable lighting source CRI, remain at low levels (Yang.X, Wang.L, J.Phys.Chem.C 2012,116,15041).Another kind of triphenylamine derivative TCTA (4 says in 2014 annual reports in Huang seminar, 4', 4 "-Tris (carbazol-9-yl)-triphenylamine; 4; 4'; 4 "-three (carbazole-9-base) triphenylamine) be the top emission type complementary colours warm white OLED of material of main part, although obtain highly stable spectral emissions, and device luminous efficiency is up to 24.5cd A
-1, but the CRI of obtained device is still the low-level (Shi.H.Y, Huang.W, Orga.Electron.2014,15,1465) being in less than 60.The problem that the CRI of the complementary colours phosphorescence white light OLED device being material of main part with triphenylamine derivative Small molecular is lower does not still make substantial breakthroughs.
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 complementary colours phosphorescence 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 DTPAFB and OXD-7, guest materials FIrpic, Ir (bt)
2(acac) form, the molecular formula of DTPAFB is as follows:
The electron transfer layer of above-mentioned complementary colours phosphorescence 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 complementary colours phosphorescence white light OLED device and the ratio of guest materials are DTPAFB:OXD-7:FIrpic:Ir (bt)
2(acac)=19:11:3:(0.09-0.12).
A preparation method for complementary colours phosphorescence 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 triphenylamine derivative small molecule host complementary colours phosphorescence white light parts 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, complementary colours phosphorescence white light OLED device CRI provided by the present invention is up to 71, be the highest level of the complementary colours white light OLED device CRI of material of main part for current triphenylamine derivative Small molecular, substantially reduce such device with the gap between desirable white-light illuminating light source.
2, triphenylamine system of the present invention derivative large-substituent group is easy for the solution processable type small molecule host material DTPAFB of skeleton has preparation, easy purification, excellent and the triplet of thermal stability, chemical stability, filming performance is up to many advantages such as 2.79eV, and the space configuration of high distortion more effectively can prevent the gathering of guest materials in luminescent layer, thus can ensure that device has metastable spectral emissions.
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, while device provided by the invention has excellent spectrum property, be 1000cd m in brightness
-2time luminous efficiency also up to 25.0cd A
-1, reach the level suitable with conventional incandescent lamp, have broad application prospects at OLED solid-state white lighting field.
5, 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 complementary colours phosphorescence white light parts structure 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 DTPAFB 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-difluorophenylpyridinato-N, C2) picolinatoiridium, two (4,6-difluorophenyl pyridinato-N, C2) pyridinecarboxylic close iridium), Ir (bt)
2(acac) (Bis (2-phenyl-benzothiazole-C2, N) (acetyl-acetonate) 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] imid-azol-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.
Wherein DTPAFB is the fragrant Small molecular that the triphenylamine system derivative large-substituent group of space structure high distortion is skeleton, and it is according to pertinent literature (Ye, S H.Liu, Y Q.Adv.Funct.Mater.2010,20,3125) the method synthesis introduced, molecular structure is as follows:
In order to prepare above-mentioned white light parts, 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, 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 (DTCPFB:OXD-7:FIrpic (19:11:3)): 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 triphenylamine derivative small molecule host complementary colours phosphorescence white light parts 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 (0.367,0.434), CCT (Correlated Colour Temperature, correlated colour temperature) be 4500K, CRI, up to 71, reaches the highest level of current similar device CRI.Excellent look quality parameter proves that 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 complementary colours phosphorescence white light parts prepared by the present invention changes with brightness.At brightness 100-10000cd 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 white light parts provided by the present invention.Can find out, the bright voltage that opens of device is 4.6V, and maximum current density is close to 550mA cm
-2, high-high brightness can reach 40000cd m
2.
As shown in Figure 5, the maximum lumen efficiency of device reaches 25.4cdA to the luminous efficiency-brightness-power efficiency characteristic curve of device
-1, be 100cd m in brightness
-2with 1000cd m
-2time, luminous efficiency is respectively 19.9cd A
-1with 25.0cd 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, 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.
The present invention, by the reasonable selection of luminescent material and the appropriate regulation of each component doping ratio, has prepared the complementary colours white light parts of high CRI, than known all complementary colours white light parts closer to the requirement of desirable lighting source.And use and the Solution processing techniques by being the organic molecule material of main part of skeleton containing large-substituent group, effectively achieve the Uniform Doped of luminescent layer component, ensure that the stability of luminescent spectrum.And have employed the exclusive device architecture type of body series from the viewpoint of the premium properties etc. that level-density parameter, carrier transport balance and selected material have self, make device reach the high efficiency suitable with conventional incandescent lamp.
Claims (10)
1. a complementary colours phosphorescence 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 DTPAFB and OXD-7, guest materials FIrpic, Ir (bt)
2(acac) form, the molecular formula of DTPAFB is as follows:
2. a kind of complementary colours phosphorescence 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 complementary colours phosphorescence white light OLED device according to claim 1, is characterized in that the ratio of material of main part and guest materials is DTPAFB:OXD-7:FIrpic:Ir (bt)
2(acac)=19:11:3:(0.09-0.12).
4. a preparation method for complementary colours phosphorescence 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 triphenylamine derivative small molecule host complementary colours phosphorescence white light parts prepared by solwution method.
5. the preparation method of a kind of complementary colours phosphorescence white light OLED device according to claim 4, it is characterized in that the step of 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 complementary colours phosphorescence 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 complementary colours phosphorescence white light OLED device according to claim 4, it is characterized in that in described step 3, 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 complementary colours phosphorescence 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 complementary colours phosphorescence 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 complementary colours phosphorescence 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109860404A (en) * | 2018-06-11 | 2019-06-07 | 南京邮电大学 | White organic LED and preparation method thereof |
| CN111384306A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Preparation method of quantum dot light-emitting diode |
| CN112993176A (en) * | 2020-12-30 | 2021-06-18 | 北京交通大学 | TADF material-based white light electroluminescent device and preparation method thereof |
-
2014
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109860404A (en) * | 2018-06-11 | 2019-06-07 | 南京邮电大学 | White organic LED and preparation method thereof |
| CN109860404B (en) * | 2018-06-11 | 2021-04-06 | 南京邮电大学 | White organic light emitting diode and preparation method thereof |
| CN111384306A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Preparation method of quantum dot light-emitting diode |
| CN111384306B (en) * | 2018-12-29 | 2021-10-29 | Tcl科技集团股份有限公司 | Preparation method of quantum dot light-emitting diode |
| CN112993176A (en) * | 2020-12-30 | 2021-06-18 | 北京交通大学 | TADF material-based white light electroluminescent device and preparation method thereof |
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Application publication date: 20150311 |