CN102097600A - Preparation method of color-tunable mixed white organic luminescent device - Google Patents
Preparation method of color-tunable mixed white organic luminescent device Download PDFInfo
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- CN102097600A CN102097600A CN2010105986485A CN201010598648A CN102097600A CN 102097600 A CN102097600 A CN 102097600A CN 2010105986485 A CN2010105986485 A CN 2010105986485A CN 201010598648 A CN201010598648 A CN 201010598648A CN 102097600 A CN102097600 A CN 102097600A
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Abstract
The invention provides a preparation method of a color-tunable mixed white organic luminescent device. The method comprises the following steps: by using a transparent thin film of an indium tin oxide semiconductor on a glass substrate as an anode, dissolving a dopant carrier and different colored phosphorescent dopants respectively in an organic solvent for a yellow phosphorescent light-emitting layer; dissolving vacancy transport substances and electronic transport substances with P-type and N-type dopants respectively in the organic solvent; depositing a vacancy excitation layer, a vacancy transport layer, the yellow light-emitting layer and an electron transport layer through a spin coating method; crosslinking various organic layers deposited by spin coating through a heating method; preparing a transparent cathode through a vacuum thermal evaporation method; depositing the electron transport layer, a blue phosphorescent light-emitting layer and the vacancy transport layer through the vacuum thermal evaporation method; depositing a reflecting anode through a magnetron sputtering method; and regulating a resistor connected in series with a blue phosphorescent transport layer through a slide-wire rheostat. The method ensures the preparation process to be simple and is beneficial to mass production, thereby reducing the cost.
Description
Technical field
The present invention relates to a kind of preparation method of luminescent device, particularly relate to a kind of preparation method of adjustable mixture of colours white organic light emitting device.
Background technology
(OLED0 is as a kind of novel organic luminescent device, has efficiently, and advantage such as simple in structure and substrate adaptability is good is acknowledged as and a kind ofly can represents 21 century to throw light on and the novel light-emitting device of Display Technique trend for Organic Light Emitting Diode.Organic luminescent device basic structure is multi-layered type, generally comprise electron transfer layer, emission layer, hole transmission layer etc., and structure is quite important aspect raising luminous efficiency and stability, has been current organic light-emitting device developing direction as the doping type structure.
The Organic Light Emitting Diode technical development can be divided into two big application directions so far substantially, and a class is to be used for flat panel display, to replace liquid crystal and plasma panel display; Another kind of is to be used for white-light illuminating, to replace existing incandescent lamp, traditional lighting lamps such as fluorescent lamp.Be used for white-light illuminating for the Organic Light Emitting Diode technology, present major technique bottleneck is efficient and life-span.Want and the competition of conventional lighting, the efficient of Organic Light Emitting Diode white-light illuminating device and colour temperature should reach 100lm/w respectively and greater than 5000k (when brightness is 1000cd/m
2The time, L
70(brightness decay be initial value 70%) life-span is 50000 hours.The index of now best Organic Light Emitting Diode white light parts is respectively: efficient 45lm/w, colour temperature 3000k, 5000 hours L70 life-spans.As seen Organic Light Emitting Diode also has suitable distance from the white-light illuminating device that becomes a kind of maturation, and especially also there is a big difference apart from practicability the life-span.The present invention proposes the adjustable mixture of colours white organic light emitting device structure of a kind of novel long-life and can break through above-mentioned bottleneck pointedly.The major technique characteristics are: adopt a kind of novel OLED structure, a transparency electrode is used as the common negative electrode of fluorescent material layer and phosphor material layer, makes independent control flows become possibility through the current density of fluorescence coating and phosphorescent layer; Phosphorescent layer is in parallel with fluorescence coating, make phosphorescent layer do not need to bear fluorescence coating required than high current density, thereby avoid the damage of phosphor material; Control the luminosity of fluorescence coating by the current density of regulating in the fluorescence coating, thereby change the ratio of fluorescence radiation in whole white light, make the temperature that is emitted white light change.The present invention compares with the conventional white light OLED structure, has the long-life, high efficiency and characteristic of simple structure.Particularly realize the variation of white light temperature by the intensity that changes fluorescence radiation, to the practical application of white light organic luminous illuminating device, meaningful especially.
Bibliographical information adopts individual layer doped polymer (MEH-PPV mixes among the PFO), can realize white light emission, and its maximal efficiency reaches about 12.6lm/w (when brightness is 1000cd/m2).To existing document and patent retrieval, find to use fluorescence coating in parallel with phosphorescent layer and realize that by change fluorescence coating luminous intensity efficient white light emission and white light colour temperature are adjustable.
Summary of the invention
It is in parallel with phosphorescent layer and realize efficient white light emission and the adjustable method of white light colour temperature by changing the fluorescence coating luminous intensity to the invention provides a kind of new use fluorescence coating, and its preparation technology is simple, reduces cost thereby be beneficial to large-scale production.The white organic light emitting device efficient height of this prepared, power efficiency reaches 20lm/w; White light quality height, colour temperature reaches 3500k; L
70Life-span is 10000 hours.Colour temperature can be adjustable between 2000-3500k.
The invention provides a kind of preparation method of adjustable mixture of colours white organic light emitting device, it is characterized in that, may further comprise the steps:
A) be anode with the indium tin oxide semiconductor hyaline membrane film on the glass substrate, and clean, dry up through ultrasonic cleaning machine;
B), be dissolved in alloy carrier and phosphorescent dopant of all kinds in the organic solvent respectively for the yellow phosphorescence luminescent layer; Thing and electric transmission thing and p type and n type alloy are transmitted in the room to be dissolved in the organic solvent respectively;
C) adopt the method deposition room excitation layer that revolves plating, room transport layer, Yellow light emitting layer and electron transfer layer;
D) the various organic layers that revolve plated deposition adopt the method for heating to carry out crosslinked;
E) adopt the method for vacuum thermal evaporation to prepare transparent cathode;
F) adopt the method for vacuum thermal evaporation to deposit electron transfer layer, blue luminescence layer and room transport layer;
G) the method deposition of reflective anode of employing magnetron sputtering;
H) adopt slide-wire rheostat to regulate the resistance of connecting with the blue-fluorescence emission layer.
Described indium tin oxide semiconductor hyaline membrane film, resistivity is 5x10
-4(ohm cm), thickness are 100 nanometers.
Described alloy carrier is 4,4 ', 4 " three (carbazole-9-yl) triphenylamines; Described phosphorescent dopant closes iridium for two [(2-methyldiphenyl and quinoxaline) acetylacetone,2,4-pentanedione] closes iridium and three (2-phenylpyridine); Described room transmission thing and electric transmission thing and p type and n type alloy are dissolved in the organic solvent respectively and are meant: respectively with 2, two [3-(the nitrogen n-formyl sarcolysine phenyl amino) phenyl] biphenyl and 2 of 2-, 3,5,6-tetrafluoro-7,7 ', 8,8 '-four cyanogen dimethyl 1,4-benzoquinone are dissolved in the oxolane, respectively with 1,3,5-three [(3-pyridine radicals)-3-phenyl] benzene and cesium carbonate are dissolved in oxolane and the ethylene glycol monoethyl ether.
The method deposition room excitation layer of plating is revolved in described employing, the room transport layer, Yellow light emitting layer and electron excitation layer are meant: will gather 3,4-ethene dioxythiophene/polystyrolsulfon acid is deposited on the indium tin oxide transparent conductive semiconductor film film as the room excitation layer; With 2, two [3-(the nitrogen n-formyl sarcolysine phenyl amino) phenyl] biphenyl and 2,3,5 of 2-, 6-tetrafluoro-7,7 ', 8,8 '-four cyanogen dimethyl 1,4-benzoquinone mixed liquors are deposited on the polystyrolsulfon acid as the room transport layer; With 4,4 ', 4 " two [(2-methyldiphenyl and the quinoxaline) acetylacetone,2,4-pentanedione] of three (carbazole-9-yl) triphenylamines and different proportion closes iridium and three (2-phenylpyridine) and closes the iridium mixed liquor and be deposited on the transport layer of room as the Yellow light emitting layer; With 1,3,5-three [(3-pyridine radicals)-3-phenyl] benzene and cesium carbonate mixed liquor are deposited on the Yellow light emitting layer as the electron excitation layer; The rotating speed that revolves plating is 2000rpm, and the time is 20 seconds.
The described various organic layers that revolve plated deposition adopt the method for heating to carry out crosslinked being meant: under deposition before the thin film, various revolve coating all 120 ℃ down heating carried out crosslinked in 15 minutes.
The method of described employing vacuum thermal evaporation prepares transparent cathode and is meant: adopting the silver-plated deposition rate of vacuum vapour deposition is 18 nm/minute, and thickness is 90 nanometers.
Method deposition electron transfer layer, blue luminescence layer and the room transport layer of described employing vacuum thermal evaporation are meant: adopt the method for vacuum thermal evaporation to deposit 30 nanometer Alq
3As electron transfer layer, 30 nanometer TPBi are as the blue luminescence layer, and 40 nanometer NPB are as the room transport layer, and deposition rate is 10 nm/minute.
The method deposition of reflective anode of described employing magnetron sputtering is meant: adopt the method for magnetron sputtering to deposit 100 nano-ITO films, power 150w, deposition rate 10 nm/minute; On ITO, deposit 20 Nano Silvers (Ag) as reflectance coating, deposition rate 20 nm/minute.
Described employing slide-wire rheostat is regulated the resistance of connecting with the blue-fluorescence emission layer and is meant: the resistance of connecting with the blue-fluorescence emission layer changes between 0.1-0.16M.
Major advantage of the present invention is:
1. the life-span is long.Because for blue fluorescent material, at current density 20mA/cm
2Condition under, can obtain satisfied luminous intensity, and this current strength is to phosphor material and Yan Taigao, working current density red, green phosphor material is about 5mA/cm
2High current intensity can damage phosphor material, thereby reduces the life-span.Use the fluorescence structure in parallel, can control fluorescence and phosphorescent layer electric current separately, make the required big electric current of fluorescence coating need not flow through phosphorescent layer, thereby significantly improve organic light-emitting device life period with phosphor material.
2. variable color temperature.Adopt the common negative electrode of a transparency electrode, adopt a transformable resistance simultaneously, thereby the change that realizes blue emission intensity is to change the temperature of white light with the flow through electric current of fluorescence coating of adjusting as fluorescence coating and phosphorescent layer.
3. high brightness.Because control flows is crossed the electric current of yellow phosphorescence layer and blue fluorescent body respectively, make phosphorescent layer and fluorescence coating can both under recommended current, work and do not damage device lifetime, therefore reached high brightness.
4. efficient height.Employing has the non-conjugated polymeric thing of high triple exciton levels as the alloy carrier, is convenient to exciton energy and is transferred to alloy from polymer support, thereby improve Yellow light emitting efficient.
5. Heat stability is good.Because the every tunic in outstanding plating back all carries out crosslinking Treatment, makes the thermal stability of composite membrane greatly increase.
6. lower driving voltage.Owing to respectively room transferring material and electron transport material are carried out p type and the doping of n type, and, make device drive voltage reduce with gold-tinted phosphorescent layer and the parallel connection of blue light phosphorescent layer.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provide detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
With indium tin oxide semiconductor hyaline membrane (ITO) film on the glass substrate is anode, and through acetone, absolute ethyl alcohol, deionized water are cleaned in ultrasonic cleaning machine, dry up.
Respectively 98 milligrams of 3DTAPBP and 5 milligrams of F4-TCNQ are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of F4-TCNQ solution and it mixed with 3DTAPBP solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.98 milligrams of TCTA are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.With 5 milligrams of Ir (MDQ)
2(acac)
2And Ir (ppy)
3, be dissolved in respectively in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 1 milliliter of Ir (MDQ) respectively
2(acac)
2And Ir (ppy)
3Solution, and it is mixed with TCTA solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Respectively with 98 milligrams of BmPyPB and 5 milligrams of cesium carbonate (Cs
2CO
3) be dissolved in 5 milliliters of oxolanes (THF) and the 10 milliliters of ethylene glycol monoethyl ethers (2-ethoxyethanol), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of cesium carbonate (Cs
2CO
3) solution and it is mixed with BmPyPB solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 5 milliliters poly-3,4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) revolves after the filtration and is plated on the ito anode as the room excitation layer, and 120 ℃ of heating 30 minutes down.Then 3DTAPBP and F4-TCNQ mixed liquor are revolved and are plated in 3, on 4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) film as the room transport layer, and 120 ℃ of heating 15 minutes down.With TCTA and Ir (MDQ)
2(acac)
2, Ir (ppy)
3Mixed liquor revolves and is plated on the transport layer of room as the Yellow light emitting layer, and 120 ℃ of heating 15 minutes down.With BmPyPB and Cs
2CO
3Mixed liquor revolves and is plated on the Yellow light emitting layer as electron transfer layer, and 120 ℃ of heating 15 minutes down.Adopt the method for vacuum thermal evaporation on electron transfer layer, to deposit 20 nano aluminum (Al) as transparent common negative electrode.On common negative electrode, adopt the method for vacuum thermal evaporation to deposit 30 nanometer Alq
3, 30 nanometer TPBi and 40 nanometer NPB are respectively as electron transfer layer, blue luminescence layer and room transport layer.Use template at last, adopt the method for magnetron sputtering on the transport layer of room, to deposit 100 nano indium tin oxide semiconductor hyaline membranes (ITO) and 20 silver of receiving (Ag) respectively, form the organic luminescent device of 6 millimeters of 6 millimeters x as reflection anode.Use slide-wire rheostat, make that the resistance of connecting with blue fluorescent body is 0.1M ohm.
Embodiment 2
With indium tin oxide semiconductor hyaline membrane (ITO) film on the glass substrate is anode, and through acetone, absolute ethyl alcohol, deionized water are cleaned in ultrasonic cleaning machine, dry up.
Respectively 98 milligrams of 3DTAPBP and 5 milligrams of F4-TCNQ are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of F4-TCNQ solution and it mixed with 3DTAPBP solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.98 milligrams of TCTA are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.With 5 milligrams of Ir (MDQ)
2(acac)
2And Ir (ppy)
3, be dissolved in respectively in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 1 milliliter of Ir (MDQ) respectively
2(acac)
2And Ir (ppy)
3Solution, and it is mixed with TCTA solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Respectively with 98 milligrams of BmPyPB and 5 milligrams of cesium carbonate (Cs
2CO
3) be dissolved in 5 milliliters of oxolanes (THF) and the 10 milliliters of ethylene glycol monoethyl ethers (2-ethoxyethanol), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of cesium carbonate (Cs
2CO
3) solution and it is mixed with BmPyPB solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 5 milliliters poly-3,4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) revolves after the filtration and is plated on the ito anode as the room excitation layer, and 120 ℃ of heating 30 minutes down.Then 3DTAPBP and F4-TCNQ mixed liquor are revolved and are plated in 3, on 4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) film as the room transport layer, and 120 ℃ of heating 15 minutes down.With TCTA and Ir (MDQ)
2(acac)
2, Ir (ppy)
3Mixed liquor revolves and is plated on the transport layer of room as the Yellow light emitting layer, and 120 ℃ of heating 15 minutes down.With BmPyPB and Cs
2CO
3Mixed liquor revolves and is plated on the Yellow light emitting layer as electron transfer layer, and 120 ℃ of heating 15 minutes down.Adopt the method for vacuum thermal evaporation on electron transfer layer, to deposit 20 nano aluminum (Al) as transparent common negative electrode.On common negative electrode, adopt the method for vacuum thermal evaporation to deposit 30 nanometer Alq
3, 30 nanometer TPBi and 40 nanometer NPB are respectively as electron transfer layer, blue luminescence layer and room transport layer.Use template at last, adopt the method for magnetron sputtering on the transport layer of room, to deposit 100 nano indium tin oxide semiconductor hyaline membranes (ITO) and 20 silver of receiving (Ag) respectively, form the organic luminescent device of 6 millimeters of 6 millimeters x as reflection anode.Use slide-wire rheostat, make that the resistance of connecting with blue fluorescent body is 0.15M ohm.
Embodiment 3
With indium tin oxide semiconductor hyaline membrane (ITO) film on the glass substrate is anode, and through acetone, absolute ethyl alcohol, deionized water are cleaned in ultrasonic cleaning machine, dry up.
Respectively 98 milligrams of 3DTAPBP and 5 milligrams of F4-TCNQ are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of F4-TCNQ solution and it mixed with 3DTAPBP solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.98 milligrams of TCTA are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.With 5 milligrams of Ir (MDQ)
2(acac)
2And Ir (ppy)
3, be dissolved in respectively in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 1 milliliter of Ir (MDQ) respectively
2(acac)
2With 2 milliliters of Ir (ppy)
3Solution, and it is mixed with TCTA solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Respectively with 98 milligrams of BmPyPB and 5 milligrams of cesium carbonate (Cs
2CO
3) be dissolved in 5 milliliters of oxolanes (THF) and the 10 milliliters of ethylene glycol monoethyl ethers (2-ethoxyethanol), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of cesium carbonate (Cs
2CO
3) solution and it is mixed with BmPyPB solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 5 milliliters poly-3,4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) revolves after the filtration and is plated on the ito anode as the room excitation layer, and 120 ℃ of heating 30 minutes down.Then 3DTAPBP and F4-TCNQ mixed liquor are revolved and are plated in 3, on 4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) film as the room transport layer, and 120 ℃ of heating 15 minutes down.With TCTA and Ir (MDQ)
2(acac)
2, Ir (ppy)
3Mixed liquor revolves and is plated on the transport layer of room as the Yellow light emitting layer, and 120 ℃ of heating 15 minutes down.With BmPyPB and Cs
2CO
3Mixed liquor revolves and is plated on the Yellow light emitting layer as electron transfer layer, and 120 ℃ of heating 15 minutes down.Adopt the method for vacuum thermal evaporation on electron transfer layer, to deposit 20 nano aluminum (Al) as transparent common negative electrode.On common negative electrode, adopt the method for vacuum thermal evaporation to deposit 30 nanometer Alq
3, 30 nanometer TPBi and 40 nanometer NPB are respectively as electron transfer layer, blue luminescence layer and room transport layer.Use template at last, the method for employing magnetron sputtering deposits 100 nano indium tin oxide semiconductor hyaline membranes (ITO) and 20 nanometers respectively on the transport layer of room silver (Ag) forms the organic luminescent device of 6 millimeters of 6 millimeters x as reflection anode.Use slide-wire rheostat, make that the resistance of connecting with blue fluorescent body is 0.1M ohm.
Embodiment 4
With indium tin oxide semiconductor hyaline membrane (ITO) film on the glass substrate is anode, and through acetone, absolute ethyl alcohol, deionized water are cleaned in ultrasonic cleaning machine, dry up.
Respectively 98 milligrams of 3DTAPBP and 5 milligrams of F4-TCNQ are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of F4-TCNQ solution and it mixed with 3DTAPBP solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.98 milligrams of TCTA are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.With 5 milligrams of Ir (MDQ)
2(acac)
2And Ir (ppy)
3, be dissolved in respectively in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 1 milliliter of Ir (MDQ) respectively
2(acac)
2With 2 milliliters of Ir (ppy)
3Solution, and it is mixed with TCTA solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Respectively with 98 milligrams of BmPyPB and 5 milligrams of cesium carbonate (Cs
2CO
3) be dissolved in 5 milliliters of oxolanes (THF) and the 10 milliliters of ethylene glycol monoethyl ethers (2-ethoxyethanol), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of cesium carbonate (Cs
2CO
3) solution and it is mixed with BmPyPB solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 5 milliliters poly-3,4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) revolves after the filtration and is plated on the ito anode as the room excitation layer, and 120 ℃ of heating 30 minutes down.Then 3DTAPBP and F4-TCNQ mixed liquor are revolved and are plated in 3, on 4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) film as the room transport layer, and 120 ℃ of heating 15 minutes down.With TCTA and Ir (MDQ)
2(acac)
2, Ir (ppy)
3Mixed liquor revolves and is plated on the transport layer of room as the Yellow light emitting layer, and 120 ℃ of heating 15 minutes down.With BmPyPB and Cs
2CO
3Mixed liquor revolves and is plated on the Yellow light emitting layer as electron transfer layer, and 120 ℃ of heating 15 minutes down.Adopt the method for vacuum thermal evaporation on electron transfer layer, to deposit 20 nano aluminum (Al) as transparent common negative electrode.On common negative electrode, adopt the method for vacuum thermal evaporation to deposit 30 nanometer Alq
3, 30 nanometer TPBi and 40 nanometer NPB are respectively as electron transfer layer, blue luminescence layer and room transport layer.Use template at last, the method for employing magnetron sputtering deposits 100 nano indium tin oxide semiconductor hyaline membranes (ITO) and 20 nanometers respectively on the transport layer of room silver (Ag) forms the organic luminescent device of 6 millimeters of 6 millimeters x as reflection anode.Use slide-wire rheostat, make that the resistance of connecting with blue fluorescent body is 0.15M ohm.
Embodiment 5
With indium tin oxide semiconductor hyaline membrane (ITO) film on the glass substrate is anode, and through acetone, absolute ethyl alcohol, deionized water are cleaned in ultrasonic cleaning machine, dry up.
Respectively 98 milligrams of 3DTAPBP and 5 milligrams of F4-TCNQ are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of F4-TCNQ solution and it mixed with 3DTAPBP solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.98 milligrams of TCTA are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.With 5 milligrams of Ir (MDQ)
2(acac)
2And Ir (ppy)
3, be dissolved in respectively in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 2 milliliters of Ir (MDQ) respectively
2(acac)
2With 1 milliliter of Ir (ppy), 3 solution, and it is mixed with TCTA solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Respectively with 98 milligrams of BmPyPB and 5 milligrams of cesium carbonate (Cs
2CO
3) be dissolved in 5 milliliters of oxolanes (THF) and the 10 milliliters of ethylene glycol monoethyl ethers (2-ethoxyethanol), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of cesium carbonate (Cs
2CO
3) solution and it is mixed with BmPyPB solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 5 milliliters poly-3,4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) revolves after the filtration and is plated on the ito anode as the room excitation layer, and 120 ℃ of heating 30 minutes down.Then 3DTAPBP and F4-TCNQ mixed liquor are revolved and are plated in 3, on 4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) film as the room transport layer, and 120 ℃ of heating 15 minutes down.With TCTA and Ir (MDQ)
2(acac)
2, Ir (ppy)
3Mixed liquor revolves and is plated on the transport layer of room as the Yellow light emitting layer, and 120 ℃ of heating 15 minutes down.With BmPyPB and Cs
2CO
3Mixed liquor revolves and is plated on the Yellow light emitting layer as electron transfer layer, and 120 ℃ of heating 15 minutes down.Adopt the method for vacuum thermal evaporation on electron transfer layer, to deposit 20 nano aluminum (Al) as transparent common negative electrode.On common negative electrode, adopt the method for vacuum thermal evaporation to deposit 30 nanometer Alq
3, 30 nanometer TPBi and 40 nanometer NPB are respectively as electron transfer layer, blue luminescence layer and room transport layer.Use template at last, the method for employing magnetron sputtering deposits 100 nano indium tin oxide semiconductor hyaline membranes (ITO) and 20 nanometers respectively on the transport layer of room silver (Ag) forms the organic luminescent device of 6 millimeters of 6 millimeters x as reflection anode.Use slide-wire rheostat, make that the resistance of connecting with blue fluorescent body is 0.1M ohm.
Embodiment 6
With indium tin oxide semiconductor hyaline membrane (ITO) film on the glass substrate is anode, and through acetone, absolute ethyl alcohol, deionized water are cleaned in ultrasonic cleaning machine, dry up.
Respectively 98 milligrams of 3DTAPBP and 5 milligrams of F4-TCNQ are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of F4-TCNQ solution and it mixed with 3DTAPBP solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.98 milligrams of TCTA are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.With 5 milligrams of Ir (MDQ)
2(acac)
2And Ir (ppy)
3, be dissolved in respectively in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 2 milliliters of Ir (MDQ) respectively
2(acac)
2With 1 milliliter of Ir (ppy), 3 solution, and it is mixed with TCTA solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Respectively with 98 milligrams of BmPyPB and 5 milligrams of cesium carbonate (Cs
2CO
3) be dissolved in 5 milliliters of oxolanes (THF) and the 10 milliliters of ethylene glycol monoethyl ethers (2-ethoxyethanol), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of cesium carbonate (Cs
2CO
3) solution and it is mixed with BmPyPB solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 5 milliliters poly-3,4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) revolves after the filtration and is plated on the ito anode as the room excitation layer, and 120 ℃ of heating 30 minutes down.Then 3DTAPBP and F4-TCNQ mixed liquor are revolved and are plated in 3, on 4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) film as the room transport layer, and 120 ℃ of heating 15 minutes down.With TCTA and Ir (MDQ)
2(acac)
2, Ir (ppy)
3Mixed liquor revolves and is plated on the transport layer of room as the Yellow light emitting layer, and 120 ℃ of heating 15 minutes down.With BmPyPB and Cs
2CO
3Mixed liquor revolves and is plated on the Yellow light emitting layer as electron transfer layer, and 120 ℃ of heating 15 minutes down.Adopt the method for vacuum thermal evaporation on electron transfer layer, to deposit 20 nano aluminum (Al) as transparent common negative electrode.On common negative electrode, adopt the method for vacuum thermal evaporation to deposit 30 nanometer Alq
3, 30 nanometer TPBi and 40 nanometer NPB are respectively as electron transfer layer, blue luminescence layer and room transport layer.Use template at last, the method for employing magnetron sputtering deposits 100 nano indium tin oxide semiconductor hyaline membranes (ITO) and 20 nanometers respectively on the transport layer of room silver (Ag) forms the organic luminescent device of 6 millimeters of 6 millimeters x as reflection anode.Use slide-wire rheostat, make that the resistance of connecting with blue fluorescent body is 0.15M ohm.
Embodiment 7
With indium tin oxide semiconductor hyaline membrane (ITO) film on the glass substrate is anode, and through acetone, absolute ethyl alcohol, deionized water are cleaned in ultrasonic cleaning machine, dry up.
Respectively 98 milligrams of 3DTAPBP and 5 milligrams of F4-TCNQ are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of F4-TCNQ solution and it mixed with 3DTAPBP solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.98 milligrams of TCTA are dissolved in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.With 5 milligrams of Ir (MDQ)
2(acac)
2And Ir (ppy)
3, be dissolved in respectively in 5 milliliters of oxolanes (THF), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 1 milliliter of Ir (MDQ) respectively
2(acac)
2And Ir (ppy)
3Solution, and it is mixed with TCTA solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Respectively with 98 milligrams of BmPyPB and 5 milligrams of cesium carbonate (Cs
2CO
3) be dissolved in 5 milliliters of oxolanes (THF) and the 10 milliliters of ethylene glycol monoethyl ethers (2-ethoxyethanol), with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.Get 2 milliliters of cesium carbonate (Cs
2CO
3) solution and it is mixed with BmPyPB solution, after the mixing with solution in ultrasonic cleaning machine ultrasonic 15 minutes with accelerate dissolution.
Get 5 milliliters poly-3,4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) revolves after the filtration and is plated on the ito anode as the room excitation layer, and 120 ℃ of heating 30 minutes down.Then 3DTAPBP and F4-TCNQ mixed liquor are revolved and are plated in 3, on 4-ethene dioxythiophene/polystyrolsulfon acid (PEDOT-PSS) film as the room transport layer, and 120 ℃ of heating 15 minutes down.With TCTA and Ir (MDQ)
2(acac)
2, Ir (ppy)
3Mixed liquor revolves and is plated on the transport layer of room as the Yellow light emitting layer, and 120 ℃ of heating 15 minutes down.With BmPyPB and Cs
2CO
3Mixed liquor revolves and is plated on the Yellow light emitting layer as electron transfer layer, and 120 ℃ of heating 15 minutes down.Adopt the method for vacuum thermal evaporation on electron transfer layer, to deposit 20 nano aluminum (Al) as transparent common negative electrode.On common negative electrode, adopt the method for vacuum thermal evaporation to deposit 30 nanometer Alq
3, 30 nanometer TPBi and 40 nanometer NPB are respectively as electron transfer layer, blue luminescence layer and room transport layer.Use template at last, the method for employing magnetron sputtering deposits 100 nano indium tin oxide semiconductor hyaline membranes (ITO) and 20 nanometers respectively on the transport layer of room silver (Ag) forms the organic luminescent device of 6 millimeters of 6 millimeters x as reflection anode.Use slide-wire rheostat, make that the resistance of connecting with blue fluorescent body is 0.25M ohm.
To the evaluation of organic luminescent device luminescent properties, comprise that to its electroluminescence spectrum CIE coordinate, current-voltage and light intensity-voltage characteristic, used equipment are Spectrascan PR650 spectrometer and Keithley 2400 digital source tables, and measure at normal temperatures.
The organic luminescent device of table 1 embodiment 1-7 brightness and power-efficient at room temperature
| The embodiment numbering | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| High-high brightness (cd/m 2) | ?30500 | 26200 | 17230 | 38450 | 22300 | 16540 | 21500 |
| Power-efficient (lm/w) | ?20.2 | 17.2 | 16.9 | 16.4 | 16.1 | 15.8 | 15.2 |
| Colour temperature (k) | ?3500 | 3000 | 3200 | 2900 | 2500 | 2600 | 2300 |
| L 70Life-span | ?10200 | 9200 | 9100 | 8300 | 6500 | 7400 | 3200 |
The white-light organic light-emitting illuminating device of present embodiment preparation, brightness is big, and the power-efficient height is tested under atmospheric conditions and under the room temperature, can reach 38000cd/m respectively
2And 20.2lm/w.The quality height that emits white light, colour temperature reaches 3500k, and the life-span is long, its L
70Life-span is up to 1000 hours.The alternative traditional lighting power supply of white organic light emitting device of this method preparation is used for white-light illuminating.
Claims (9)
1. the preparation method of adjustable mixture of colours white organic light emitting device is characterized in that, may further comprise the steps:
A) be anode with the indium tin oxide semiconductor hyaline membrane film on the glass substrate, and clean, dry up through ultrasonic cleaning machine;
B), be dissolved in alloy carrier and phosphorescent dopant of all kinds in the organic solvent respectively for the yellow phosphorescence luminescent layer; Thing and electric transmission thing and p type and n type alloy are transmitted in the room to be dissolved in the organic solvent respectively;
C) adopt the method deposition room excitation layer that revolves plating, room transport layer, Yellow light emitting layer and electron transfer layer;
D) the various organic layers that revolve plated deposition adopt the method for heating to carry out crosslinked;
E) adopt the method for vacuum thermal evaporation to prepare transparent cathode;
F) adopt the method for vacuum thermal evaporation to deposit electron transfer layer, blue luminescence layer and room transport layer;
G) the method deposition of reflective anode of employing magnetron sputtering;
H) adopt slide-wire rheostat to regulate the resistance of connecting with the blue-fluorescence emission layer.
2. the preparation method of adjustable mixture of colours white organic light emitting device according to claim 1 is characterized in that, described indium tin oxide semiconductor hyaline membrane film, and resistivity is 5x10
-4(ohm cm), thickness are 100 nanometers.
3. the preparation method of adjustable mixture of colours white organic light emitting device according to claim 1 is characterized in that, described alloy carrier is 4,4 ' and, 4 " three (carbazole-9-yl) triphenylamines; Described phosphorescent dopant closes iridium for two [(2-methyldiphenyl and quinoxaline) acetylacetone,2,4-pentanedione] closes iridium and three (2-phenylpyridine); Described room transmission thing and electric transmission thing and p type and n type alloy are dissolved in the organic solvent respectively and are meant: respectively with 2, two [3-(the nitrogen n-formyl sarcolysine phenyl amino) phenyl] biphenyl and 2 of 2-, 3,5,6-tetrafluoro-7,7 ', 8,8 '-four cyanogen dimethyl 1,4-benzoquinone are dissolved in the oxolane, respectively with 1,3,5-three [(3-pyridine radicals)-3-phenyl] benzene and cesium carbonate are dissolved in oxolane and the ethylene glycol monoethyl ether.
4. the preparation method of adjustable mixture of colours white organic light emitting device according to claim 1, it is characterized in that, the method deposition room excitation layer of plating is revolved in described employing, the room transport layer, Yellow light emitting layer and electron excitation layer are meant: will gather 3,4-ethene dioxythiophene/polystyrolsulfon acid is deposited on the indium tin oxide transparent conductive semiconductor film film as the room excitation layer; With 2, two [3-(the nitrogen n-formyl sarcolysine phenyl amino) phenyl] biphenyl and 2,3,5 of 2-, 6-tetrafluoro-7,7 ', 8,8 '-four cyanogen dimethyl 1,4-benzoquinone mixed liquors are deposited on the polystyrolsulfon acid as the room transport layer; With 4,4 ', 4 " two [(2-methyldiphenyl and the quinoxaline) acetylacetone,2,4-pentanedione] of three (carbazole-9-yl) triphenylamines and different proportion closes iridium and three (2-phenylpyridine) and closes the iridium mixed liquor and be deposited on the transport layer of room as the Yellow light emitting layer; With 1,3,5-three [(3-pyridine radicals)-3-phenyl] benzene and cesium carbonate mixed liquor are deposited on the Yellow light emitting layer as the electron excitation layer; The rotating speed that revolves plating is 2000rpm, and the time is 20 seconds.
5. the preparation method of adjustable mixture of colours white organic light emitting device according to claim 1, it is characterized in that, the described various organic layers that revolve plated deposition adopt the method for heating to carry out crosslinked being meant: under deposition before the thin film, various revolve coating all 120 ℃ down heating carried out crosslinked in 15 minutes.
6. the preparation method of adjustable mixture of colours white organic light emitting device according to claim 1, it is characterized in that, the method of described employing vacuum thermal evaporation prepares transparent cathode and is meant: adopting the silver-plated deposition rate of vacuum vapour deposition is 18 nm/minute, and thickness is 90 nanometers.
7. the preparation method of adjustable mixture of colours white organic light emitting device according to claim 1, it is characterized in that method deposition electron transfer layer, blue luminescence layer and the room transport layer of described employing vacuum thermal evaporation are meant: adopt the method for vacuum thermal evaporation to deposit 30 nanometer Alq
3As electron transfer layer, 30 nanometer TPBi are as the blue luminescence layer, and 40 nanometer NPB are as the room transport layer, and deposition rate is 10 nm/minute.
8. the preparation method of adjustable mixture of colours white organic light emitting device according to claim 1, it is characterized in that, the method deposition of reflective anode of described employing magnetron sputtering is meant: adopt the method for magnetron sputtering to deposit 100 nano-ITO films, power 1550w, deposition rate 10 nm/minute; On ITO, deposit 20 Nano Silvers (Ag) as reflectance coating, deposition rate 20 nm/minute.
9. the preparation method of adjustable mixture of colours white organic light emitting device according to claim 1, it is characterized in that described employing slide-wire rheostat is regulated the resistance of connecting with the blue-fluorescence emission layer and is meant: the resistance of connecting with the blue-fluorescence emission layer changes between 0.1-0.16M.
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