CN101814587A - Method for improving coupling luminous efficiency of flat plate luminescent device - Google Patents
Method for improving coupling luminous efficiency of flat plate luminescent device Download PDFInfo
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- CN101814587A CN101814587A CN 201010143598 CN201010143598A CN101814587A CN 101814587 A CN101814587 A CN 101814587A CN 201010143598 CN201010143598 CN 201010143598 CN 201010143598 A CN201010143598 A CN 201010143598A CN 101814587 A CN101814587 A CN 101814587A
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Abstract
The invention belongs to the field of flat plate luminescent devices, in particular to the field of organic electroluminescent devices, and relates to a method for improving the coupling luminous efficiency of the flat plate luminescent device, in particular to a method for improving the coupling luminous efficiency of the flat plate luminescent device by preparing a nano-cone array on the surface of a substrate of the organic electroluminescent device through direct etching. In the method, the coupling luminous efficiency of a white organic electroluminescent device is improved by 1.4 times by using excellent broad band anti-reflection performance of the nano-cone array. Simultaneously, the ratio of the luminous intensity of one apparatus to that of another apparatus is increased by 60 times when an angle is up to 70 degrees.
Description
Technical field
The invention belongs to the flat plate luminescent device field, particularly the organic electroluminescence device field is specifically related to a kind of method that improves coupling luminous efficiency of flat plate luminescent device.
Background technology
Organic electroluminescence device belongs to injection luminescent diode, just electric energy is converted into the device of luminous energy, at first electronics and hole are injected into the organic luminous layer from two lateral electrodes respectively, charge carrier moves in organic layer under the effect of electric field outside then, compound back forms exciton, and exciton in luminescent layer radiation recombination takes place and luminous; Have from main light emission, low voltage drive, advantage such as the visual angle is wide, response is fast, color is abundant.White organic light emitting device particularly is because it can be used as the solid light source of display device of future generation and a new generation and is extensively paid close attention to.
The structure of typical organic electroluminescence device is: substrate/anode/organic luminous layer/negative electrode.Because there is bigger difference in the refractive index of every layer material, thus refraction and reflection can be formed at each place, bed boundary, when light can be produced the total reflection phenomenon of light during to the low material layer incident of refractive index by the high material layer of refractive index.Thereby the coupling luminous efficiency that causes device has only about 20%, and most light has all lost at device inside, thereby has limited the raising of electroluminescent device external quantum efficiency greatly, has hindered the practical application of electroluminescent device.
In order to address the above problem, at patent documentation (United States Patent (USP): disclose a kind of method 6984934), promptly in the substrate of organic electroluminescence device, constructed one deck microlens array and improve coupling luminous efficiency.Yet make this lenticular process more complicated, need to adopt traditional photoetching process, promptly produce template earlier, on template, make lenticule then, transfer to again in the substrate of organic electroluminescence device.In order to improve lenticular manufacture method, (Chinese patent: the substrate surface injection of mentioning publication number CN1719955A) to organic electroluminescence device contains formation microlens material and the drop low with the substrate material surface compatibility, makes drop solidify to form lenticule then at another piece patent documentation.This method technical process is fairly simple, but the drop size of spraying is difficult to control, causes at the lenticule of organic luminescent device substrate surface formation not of uniform size, very irregular.There is the lenticular complex process of making in order to improve above-mentioned technology, or the unmanageable shortcoming of lenticular size, at patent documentation (Chinese patent: ZL 2,006 10131629.5) first making microballoon has been proposed, again the microballoon through screening partly is pressed into the method that is spin-coated in advance in the suprabasil polymer of organic luminescent device, forms the class microlens structure.Whole technical process does not need photoetching, and is fairly simple comparatively speaking, and diameter of micro ball can be selected in addition, makes the class lenticule size of final formation consistent, evenly neat.But all there is a problem in said method, it is exactly the material polymeric material often of the microlens array of preparation, and with substrate be different material, so the adhesion of this microlens array and substrate is not fine, the structural-mechanical property of preparation is good inadequately.
Summary of the invention
The method that the purpose of this invention is to provide a kind of easy raising coupling luminous efficiency of flat plate luminescent device, at made the shortcoming that lenticular complex process, lenticular size are difficult to control, lenticular mechanical performance is bad in the past, proposition is in the method for the direct etching of substrate surface of organic electroluminescence device, the preparation nano-cone array, reduce light in the reflection of substrate surface, increase seeing through of light, and then restriction light improves the coupling luminous efficiency of light in the total reflection of substrate and air interface.Its glow color is not only applicable to white light, can be any light in the visible region.
To achieve the object of the present invention, technical scheme of the present invention may further comprise the steps:
(1) the preparation diameter is the microballoon of nanometer or micron dimension;
(2) side in the organic electroluminescence device transparent substrates prepares compact arranged individual layer microballoon;
(3) be mask with compact arranged individual layer microballoon, utilize the reactive ion etching technology to prepare the antireflective and the anti-reflection surface of nano-cone array in a side of transparent substrates;
(4) at the big and transparent electrode material of a side magnetron sputtering work function of the transparent substrates that does not have nano-cone array as anode layer;
(5) on anode layer, make organic polymer layers or micromolecule layer more successively, and the little electrode material of work function is as cathode layer, thus the improved flat plate luminescent device of preparation coupling luminous efficiency.
Microballoon described in the said method step (1) is inorganic material microballoon or polymeric material microballoon (for example: polystyrene microsphere, poly (methyl methacrylate) micro-sphere, silicon dioxide microsphere etc.), and diameter is 100～5000 nanometers; Organic luminescent device comprises transparent substrates, anode layer and cathode layer and is clipped in two organic polymer layers or micromolecule layers between the electrode layer, wherein the material of organic polymer layers can be selected trapezoidal polyphenyl and derivative, polyphenylene ethylene and derivative thereof, poly-fluorenes and derivative thereof etc. for use, and the material of micromolecule layer can be selected 8-hydroxyquinoline aluminum, triphenylamine and derivative thereof, phenolic group pyridine complex, quinacridone derivative, porphyrin metal complex etc. for use; Transparent substrates is used glass, quartz plate or flexiplast; The material of anode layer is that work function is big and want transparent metal, alloy or electrical conductivity compound (as tin indium oxide, zinc oxide, indium zinc oxide, gold, copper, silver etc.), and the thickness of anode layer is 100～200nm; Organic polymer layers or micromolecule layer are wherein one or more layers of hole injection layer, hole transmission layer, electronic barrier layer, luminescent layer, hole blocking layer, electron transfer layer, electron injecting layer; The material of cathode layer is the low metal or alloy of work function, and (for example, Li: the Al alloy by mass, contains 0.6% Li as the alloy of lithium metal, magnesium, calcium, strontium, aluminium or they and copper, gold, silver; Mg: Ag alloy, both mass ratioes 10: 1) etc., the thickness of cathode layer is 100～150nm.
Structure, material and the electrode of dull and stereotyped organic electroluminescence device itself are not the inventive point of this patent, about device architecture, bilayer or sandwich construction (Appl.Phys.Lett.1987,51,913) are arranged more typically.
Carry out below than specific description:
1. closely arrange the preparation of individual layer polystyrene microsphere: (wherein the polystyrene microsphere of 200～1000 nanometers is the emulsion polymerisation process preparation with the polystyrene microsphere emulsion of 200～5000 nanometers, the preparation method of polystyrene microsphere is referring to J.H.Zhang, Z.Chen, Z.L.Wang, W.Y.Zhang, N.B.Ming, Mater.Lett.2003,57,4466; 1～5 micron polystyrene microsphere is buied by ALDRICH company) after the eccentric cleaning, be that 1～2.5: 1 the absolute ethyl alcohol and the mixed solution of deionized water disperse with volume ratio, obtain mass concentration and be 0.5～2.0% polystyrene microsphere emulsion; With syringe the polystyrene microsphere emulsion of the above-mentioned concentration of 50～100 microlitres is added drop-wise to the surface of deionized water in the glass culture dish that fills deionized water slowly again, dripping 20～50 microlitre mass concentrations to the surface of deionized water again is 2.0～8.0% lauryl sodium sulfate deionized water solution;
(it is that 98% the concentrated sulfuric acid and mass concentration are the mixed solution of 30% hydrogen peroxide that the quartz plate substrate is placed mass concentration with the quartz plate substrate of cleaning surfaces and hydrophilicity-imparting treatment, the consumption volume ratio of two kinds of solution is 7: 3, boil and handled 20～30 minutes, again through dry under nitrogen or air atmosphere after the rinsed with deionized water) the individual layer polystyrene microsphere that will float over the deionized water surface picks up, after the air dry, just assembling has obtained the individual layer polystyrene microsphere on the quartz plate surface.With reference to our patent documentation (Chinese patent: publication number CN 101497429A).What be worth proposition is the method for the compact arranged individual layer microballoon of preparation, also can be that the interface picks up method, czochralski method, spin-coating method, directly evaporation, electric field are assisted methods such as assembling, trans-printing.
2. constructing of silicon dioxide nano-cone array: the reactive ion etching that the quartz plate of the compact arranged individual layer polystyrene microsphere of the surface-assembled that obtains is carried out fluorine, etching power is that RF150～400W, chamber pressure are 30～50mTorr, the tetrafluoromethane flow is 20～40SCCM, argon flow amount is 0～30SCCM, etch period is 2～100 minutes, with chloroform remaining polystyrene is removed afterwards, just obtained silicon dioxide nano-cone array, the cycle is between 100nm～5000nm.With reference to our patent documentation (Chinese patent: application number 200910217746.7).
At magnetron sputtering 100～200nm indium tin oxide transparent material of the quartz plate substrate of not carrying out etching as anode layer;
4. on anode layer, use conventional methods and make 100～200nm organic polymer or micromolecule layer, and the thick cathode layer of 100～150nm, thereby organic light-emitting device preparation of the present invention finished.
Description of drawings
Fig. 1: the electron micrograph of organic luminescent device underlying structure;
Fig. 2: the organic luminescent device schematic diagram, wherein 1 is cathode layer, the 2nd, be organic luminescence polymer layer or micromolecule layer, the 3rd, indium tin oxide, the 4th, organic light-emitting device substrate;
Fig. 3: silicon dioxide nano-cone array is arranged and do not have the standard electroluminescent spectrum of the organic electroluminescence device normal direction of silicon dioxide nano-cone array, wherein curve a is the device that silicon dioxide nano-cone array is arranged, and curve b is the device that does not have silicon dioxide nano-cone array;
Fig. 4: the ratio of organic electroluminescence device electroluminescence peak strength that silicon dioxide nano-cone array is arranged and do not have silicon dioxide nano-cone array is with the variation of observation angle, and wherein normal direction is 0 degree angle.Wherein curve a is 597.5nm, and curve b is 549.0nm, and curve c is 513.5nm, and curve d is 453.5nm;
Fig. 5: the normalized energy efficient of organic electroluminescence device normal direction that silicon dioxide nano-cone array is arranged and do not have a silicon dioxide nano-cone array is with the electric current change curve, wherein curve a is the device that silicon dioxide nano-cone array is arranged, and curve b is the device that does not have silicon dioxide nano-cone array;
Fig. 6: the brightness of organic electroluminescence device normal direction that silicon dioxide nano-cone array is arranged and do not have a silicon dioxide nano-cone array is with the electric current change curve, wherein curve a is the device that silicon dioxide nano-cone array is arranged, and curve b is the device that does not have silicon dioxide nano-cone array.
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.Should be appreciated that the present invention is not limited to following preferred implementation, preferred implementation is as just illustrative embodiment of the present invention.
Embodiment
Embodiment 1:
1. the preparation method of polystyrene microsphere:
Under nitrogen protection; with 40 milliliters absolute ethyl alcohols and 100 ml deionized water is decentralized medium; with 3.3 milliliters of styrene; 0.0733 the potassium peroxydisulfate of gram; 0.0807 the dodecyl sodium sulfate of gram; join in the reactor that mechanical agitator and reflux condensing tube are housed, mechanical agitation speed is at 350 rev/mins.Carry out polymerization reaction in 70 ℃ water-bath, react and obtain emulsion stable, milky monodisperse polystyrene microsphere after 10 hours, diameter of micro ball is 204 nanometers.
2. the preparation of compact arranged individual layer polystyrene microsphere:
With the polystyrene microsphere centrifuge washing that makes, be 1.5: 1 absolute ethyl alcohol and the dispersion of deionized water mixed solution again with volume ratio, getting solid content is the emulsion of 0.5% (mass fraction) monodisperse polystyrene microsphere, get the emulsion of 50 microlitres with syringe, be added drop-wise to the diameter that fills deionized water (200 milliliters) slowly and be in 9 centimetres the glass culture dish, drip 20 microlitre mass percentage concentration again and be the deionized water solution of 5.0% lauryl sodium sulfate; With the quartz plate substrate of handling clean and surface hydrophilic the polystyrene individual layer microballoon of keeping afloat is picked up, after the air dry, just obtained compact arranged individual layer polystyrene microsphere, thickness is 204 nanometers.
3. the preparation of silicon dioxide nano-cone array:
There is the quartz plate substrate of compact arranged individual layer polystyrene microsphere to carry out the reactive ion etching of fluorine to the surface-assembled that obtains, etching power is that RF 300W, chamber pressure are 40mTorr, the tetrafluoromethane flow is 30SCCM, argon flow amount is 20SCCM, etch period is 7 minutes, with chloroform remaining polystyrene is removed afterwards and is just obtained silicon dioxide nano-cone array, and the cycle is 204 nanometers, highly be 236 nanometers, end diameter is 190 nanometers.As shown in Figure 1.
4. the preparation of transparency electrode:
Utilizing magnetic control sputtering device is the tin indium oxide of 200 nanometers at the another side sputter thickness of the substrate with silicon dioxide nano-cone array, as anode layer.
5. the preparation of organic electroluminescence device:
Be manufactured with organic electroluminescence devices on anode layer, structure is: ITO/N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4 ,-4-diamines (being called for short NPB) is (40nm)/2,5,2 ', the basic biphenyl in 5 '-four (2, the 2-diphenylethlene) (being called for short TDPVBI) (30nm)/9,9 '-(1, the 3-phenyl) two-9H-carbazole: 8% 2-(2-(9,9 ' spiral shell two fluorenes-7)) pyridine single acetyl acetone closes erbium (III) and (is called for short (SBFP)
2Ir (acac)) (20nm)/1,3,5-three (benzene of 1-phenyl-1H-benzimidazolyl-2 radicals-yl) (being called for short TPBI) (40nm)/LiF (0.5nm)/Al (100nm), simultaneously, in order to compare explanation, in the substrate that does not have silicon dioxide nano-cone array, made the organic electroluminescence device of same structure.Above-mentioned organic electroluminescence device is to adopt the mode of thermal evaporation to make in vacuum chamber, and vacuum chamber pressure is 6 * 10
-4Pa.In this kind device architecture, NPB is a hole transmission layer, and TPBI is an electron transfer layer.As shown in Figure 2.
Fig. 3 is that the electroluminescence intensity of organic electroluminescence device normal direction that silicon dioxide nano-cone array arranged and do not have a silicon dioxide nano-cone array is with the electric current change curve.Can see that it is 1.4 times of organic electroluminescence device that do not have silicon dioxide nano-cone that the organic electroluminescence device of silicon dioxide nano-cone luminous intensity is arranged.
Fig. 4 is that the ratio of electroluminescent spectrum peak value of organic electroluminescence device that silicon dioxide nano-cone array arranged and do not have a silicon dioxide nano-cone array is with the variation of observation angle, wherein normal direction is 0 degree angle, and the device electroluminescence intensity that has structure as can be seen all is greater than the device of ordinary construction at any angle direction.And for the enhancing of the long light of ripple than wavelength short enhancing a lot of greatly, just this structure helps the enhancing for longwave optical more.When angle reaches 70 degree, two kinds of device luminous intensity ratios even reached 60 times.
Shown in Figure 5 is the curve of two device energy efficiencies and current density, is about 1.4 times of commonplace components efficient for its efficient of this device that has structure.
Shown in Figure 6 is that two kinds of device architecture standards go out luminous intensity under the light state for the curve of current density, as can be seen from the figure, the intensity of two kinds of device architectures all is to increase along with the increase of current density, yet for the device that has etching structure, its luminous intensity luminous intensity than ordinary construction device under the same conditions is high a lot.Mainly be because thisly formed a kind of structure of comparison rule, reduced when light is propagated in glass, make most of light all be coupled out, improved the light extraction efficiency of device greatly in the total reflection of surface through the quartz glass surface after the etching processing.
This method of improving coupling luminous efficiency of flat plate luminescent device, to luminescent material without limits, its glow color is not only applicable to white light, can be any light in the visible region.
Although describe the present invention in conjunction with the preferred embodiments, but the present invention is not limited to the foregoing description, should be appreciated that under the present invention conceives guiding, those skilled in the art can carry out various modifications and improvement, and claims have been summarized scope of the present invention.
Claims (8)
1. method of improving coupling luminous efficiency of flat plate luminescent device, it may further comprise the steps:
(1) the preparation diameter is the microballoon of nanometer or micron dimension;
(2) side in the organic electroluminescence device transparent substrates prepares compact arranged individual layer microballoon;
(3) be mask with compact arranged individual layer microballoon, utilize the reactive ion etching technology to prepare the antireflective and the anti-reflection surface of nano-cone array in a side of transparent substrates;
(4) at the big and transparent electrode material of a side magnetron sputtering work function of the transparent substrates that does not have silicon dioxide nano-cone array as anode layer;
(5) on anode layer, make organic polymer layers or micromolecule layer more successively, and the little electrode material of work function is as cathode layer, thus the improved flat plate luminescent device of preparation coupling luminous efficiency.
2. a kind of method of improving coupling luminous efficiency of flat plate luminescent device as claimed in claim 1 is characterized in that: be that the preparation diameter is polymer microballoon or the inorganic microsphere of 100nm～5000nm.
3. a kind of method of improving coupling luminous efficiency of flat plate luminescent device as claimed in claim 1, it is characterized in that: the side in the organic electroluminescence device transparent substrates prepares compact arranged individual layer microballoon, employing be that the interface picks up method, czochralski method, spin-coating method, directly evaporation, the auxiliary construction from part of electric field or trans-printing method.
4. a kind of method of improving coupling luminous efficiency of flat plate luminescent device as claimed in claim 1 is characterized in that: organic electroluminescence device comprise transparent substrates, anode layer, cathode layer and be clipped in anode layer and cathode layer between organic polymer layers or micromolecule layer.
5. a kind of method of improving coupling luminous efficiency of flat plate luminescent device as claimed in claim 1, it is characterized in that: the cycle of the nano-cone array of preparation is between 100nm～5000nm.
6. a kind of method of improving coupling luminous efficiency of flat plate luminescent device as claimed in claim 1 is characterized in that: transparent substrates is glass, quartz plate or flexiplast.
7. a kind of method of improving coupling luminous efficiency of flat plate luminescent device as claimed in claim 1 is characterized in that: anode layer is tin indium oxide, zinc oxide, indium zinc oxide, gold, copper or silver; Cathode layer is lithium, magnesium, calcium, strontium or aluminium, or they and copper, gold or silver-colored alloy.
8. a kind of method of improving coupling luminous efficiency of flat plate luminescent device as claimed in claim 1 is characterized in that: organic polymer layers or micromolecule layer are one or more layers in hole injection layer, hole transmission layer, electronic barrier layer, luminescent layer, hole blocking layer, electron transfer layer or the electron injecting layer.
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