CN101359722A - Encapsulation method for top radiation organic EL part - Google Patents
Encapsulation method for top radiation organic EL part Download PDFInfo
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- CN101359722A CN101359722A CNA2008100512023A CN200810051202A CN101359722A CN 101359722 A CN101359722 A CN 101359722A CN A2008100512023 A CNA2008100512023 A CN A2008100512023A CN 200810051202 A CN200810051202 A CN 200810051202A CN 101359722 A CN101359722 A CN 101359722A
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Abstract
The invention belongs to the organic electroluminescence field, in particular to a packaging method for a top-emitting organic electroluminescent device, comprising the packaging to the top-emitting organic electroluminescent device having an upright structure and an inverted structure. A layer of organic or inorganic material which has a thickness of 10nm to 100nm and has high transmittance in a visible light region and is also easy of thermal evaporation deposition is coated on a top electrode of the top-emitting organic electroluminescent device to serve as a protective layer of the device, then a luminous zone of the device is coated with package resin, and finally a transparent packaging cover plate is pressed thereon. The method improves the packaging tightness of the device, avoids the damage to the device caused by friction, and overcomes the disadvantages of complicated operational procedures, long solidification time and high costs of the previous packaging process, and the method has advantages of simple process, short solidification time, low costs and good barrier property of oxygen and vapor, and is widely applied in the aspect of packaging to electronic and electrical devices such as organic electroluminescent devices (OLED).
Description
Technical field
The invention belongs to the organic electroluminescent field, be specifically related to a kind of new top radiation organic EL part method for packing.
Background technology
Organic electroluminescence device (OLED) is a kind of novel planar display device of present development newly developed.Because OLED can satisfy people's all demands to display, promptly have self-luminous, frivolous, response speed is fast, the visual angle is wide, large scale display, low voltage and direct current drive, technology is simple, cost is low, can also realize advantages such as flexible demonstration, therefore, the Display Technique of future generation that is considered to the most desirable and tool development prospect.Present active OLED ray structure has bottom-emission and two kinds of structures of top light emitting.And then the anode ITO of end ballistic device is the OLED organic luminous layer below, is the metal or alloy negative electrode topmost.When electroluminescence, light is from the one side outgoing of ITO/ glass substrate, and when this device application was shown to active driving OLED, display device pixel-driving circuit and show the problem that light-emitting area can occur vying each other can influence the aperture opening ratio of device.And the light of top ballistic device (TEOLED) is from top electrode one side outgoing, and pixel-driving circuit etc. is produced on below the device, so just can solve device pixel-driving circuit etc. and the problem that shows that light-emitting area is vied each other, and then improved the aperture opening ratio of device.Based on above reason, top radiation organic EL part becomes a research focus in recent years.
The poor stability of early stage luminous organic material and device, make people produce suspection to its application prospect, obtained breakthrough at material aspect synthetic in recent years, half-life as green light material has reached 20000～50000h, the half-life of blue light material has also surpassed 30000h, and the luminosity of OLED has surpassed 100000cd/m
2, and made the OLED sample that full color shows.But stability and the life problems of OLED are not solved at all, and this is the main line that runs through whole OLED research.There are a plurality of factors in the stability and the life-span that influence device, but the stability of electroluminescent organic material and cathode material is the bottleneck of restriction OLED stability.
Electroluminescent organic material to oxygen and steam invade responsive especially (Ullrich M, Peter B.J MaterChem, 2000,10:1471), be on the one hand because oxygen directly is exactly the triplet state quencher, luminous quantum efficiency is significantly descended; On the other hand, oxygen generates carbonyls to the oxidation meeting of luminescent layer, this compound also be effective quencher (Sutherland D G J, Carlisle J A, Elliker P, Fox G.Appl PhysLett, 1996,68:2046); Organic layer thickness is generally less than in addition
Will form blackspot in case luminescent material is rotten, and follow luminous efficiency decline energy gap to increase; Oxygen descends its transmittability to the oxidation of hole transmission layer.The influence of steam is more obvious, and its main failure mode is the hydrolysis of conduction and organic layer compound, and stability is descended greatly.
Equally, because organic material is more much smaller than the electron affinity of metal and inorganic material among the OLED, the work function that reaches effective electric transmission cathode material must be very low, so what be used for the OLED negative electrode almost is alkali metal or alkali earth metal entirely, these active metals were both oxidized extremely easily, were hydrolyzed extremely easily again.
As everyone knows, glass can form airtight cavity fully by sintering, but with glass packaging OLED the time, the high temperature of generation is a kind of fatal infringement to device.For avoiding using sintering, can only be at glass packaging seam crossing macromolecule binding material, consequently airborne oxygen and moisture penetrate in the device from seam crossing easily, and the seal of glass packaging is descended.Someone adopts OLED is embedded in (Denki K in the liquid fluorocarbons, Kogyo K K.JP4363890.1992) or in fill out dehydrating agent (PioneerElectronic Corporation, Tohoku Pioneer Electronic Corporation.US5882761.1999).
Still there is certain defective in existing method for packing, especially the application in the full color top radiation organic EL part.In order to guarantee certain light transmission, it is very thin that the metallic cathode of top radiation organic EL part is all done usually; Simultaneously in order to realize that full color shows, the encapsulation of device to relate to color filter film to the version problem, and with existing method for packing during to version, because the existence that rubs is easy to device cathodes is caused wearing and tearing.
Summary of the invention
The method for packing that the purpose of this invention is to provide a kind of simple top radiation organic EL part.It comprises the steps:
A. make the organic electroluminescence device of top emission;
B. on the top electrode of device evaporation one deck at visible region transmitance more than 70%, the easily organic material or the inorganic material protective layer of evaporation;
C. on protective layer, apply ultra-violet curing glue;
D. the transparent enclosure cover plate is pressed onto on the ultra-violet curing glue;
E. the ultraviolet irradiation device makes the ultra-violet curing adhesive curing, finishes the encapsulation to device.
At said method, organic electroluminescence device can be traditional positive interposed structure top radiation organic EL part, also can be the inverted structure top radiation organic EL part, device architecture be generally substrate/anode/hole injection layer/hole transmission layer/luminescent layer/electron transfer layer/electron injecting layer/negative electrode top electrode; Or substrate/negative electrode/electron injecting layer/electron transfer layer/luminescent layer/hole transmission layer/hole injection layer/anode top electrode; The organic material that uses as organic function layer (hole injection layer, hole transmission layer, luminescent layer, electron transfer layer or electron injecting layer) can be that small molecule material also can be a polymeric material.
The organic material protective layer of evaporation is 4,4 '-N, N-two carbazoles-biphenyl (CBP), three (oxine) aluminium (Alq
3), N, N '-two-(1-phenyl)-N, N '-diphenyl-1,1 '-xenyl-4,4 '-diamines (NPB) or 2,9-dimethyl-4,7-diphenyl-1,10-connection phenanthroline (BCP) etc.;
The inorganic material protective layer of evaporation is MoO
3, WO
3, ReO
3, ZnO, TeO
2, ZnS or ZnSe etc.
The thickness of organic or inorganic material protection layer can be adjusted to reach the best according to the emission wavelength of top radiation organic EL part and go out light effect, and scope is generally between 10nm～100nm.
The transparent enclosure cover plate can adopt any transparent material, as simple glass sheet or polymethyl methacrylate sheet, also can be the colored filter that is used to realize the full color demonstration.
The present invention proposed before the organic electroluminescence device encapsulation; having than high permeability of first one deck suitable thickness of on device, growing at visible region; easily the organic material of thermal evaporation or inorganic material directly press the encapsulation cover plate as protective layer after ultra-violet curing glue is coated in the device luminous zone simultaneously.This method has improved the seal of device package, has avoided the device damage that causes owing to friction.
The operating procedure that method of the present invention has overcome packaging technology in the past is numerous and diverse, curing time shortcoming such as length, cost height, characteristics such as have that process is simple, curing time is short, cost is low, oxygen and water vapor barrier property are good are used having widely aspect the electric devices such as encapsulation organic electroluminescent device OLED.
Description of drawings
The encapsulation process schematic diagram of Fig. 1: TEOLED;
As shown in Figure 1,1 be silicon substrate wherein; The 2nd, the OLED device; The 3rd, organic material or inorganic material protective layer; The 4th, ultra-violet curing glue (UV glue); The 5th, the transparent enclosure cover plate, the present invention preferentially selects glass for use; The 6th, UV-irradiation.
Embodiment
Embodiment 1:
Preparation of devices is to carry out in multi-source organic molecule gas-phase deposition system, and detailed preparation process is as follows:
[1] silicon substrate is cleaned repeatedly with acetone, ethanol, deionized water successively and is ultrasonic, oven dry then;
[2] substrate of handling well is placed multi-source organic molecule gas-phase deposition system (referring to Chinese patent: ZL03110977.2, " the crucible type evaporation source that is used for the organic electroluminescent coating machine "), comprise organic evaporating area (8 evaporation sources) and evaporation of metal district (2 evaporation sources) in the same vacuum cavity of system, completely cut off mutually between two districts and between each evaporation source, avoided mutual pollution, substrate can rotate to organic evaporating district or top, evaporation of metal district respectively, make things convenient for the growth of material, substrate distance evaporation source 25cm, can rotation and revolution to guarantee the uniformity of metal film and organic membrane, material therefor is placed on respectively in the different evaporation sources of different evaporating area, the temperature of each evaporation source can be controlled separately, is evacuated to 3 * 10-4Pa then;
[3] under above-mentioned vacuum condition, the Ag that evaporation 70nm is thick on substrate earlier is as anode, again successively evaporation 45nm thick 4,4 ', 4 "-three (3-aminomethyl phenyl aniline) triphenylamine (m-MTDATA) is as hole injection layer; the N that 5nm is thick; N '-two-(1-phenyl)-N, N '-diphenyl-1,1 '-xenyl-4; 4 '-diamines (NPB) is as hole transmission layer, three (oxine) aluminium (Alq that 60nm is thick
3) as luminescent layer and electron transfer layer, the thick LiF of 1nm is as electron injecting layer, the thick Ag of last Al that evaporation 1nm is thick again and 22nm is as semitransparent cathode;
[4] again with substrate-transfer to the organic evaporating district, it is constant to keep above-mentioned vacuum condition, evaporation MoO on negative electrode
3, the speed of growth is 0.1nm/s, thickness is 30nm.
The thickness of the above material growth and growth rate are produced the control of L-400 film-thickness monitoring by the U.S., and the device performance of preparation gained is tested under the normal temperature condition in air with PR650 spectrometer and Keithley2400 current/voltage source.
MoO has grown
3Behind the film, device is put into the Braun glove box, be coated with last layer ultra-violet curing glue in the luminous zone of device earlier, the model of ultra-violet curing glue is star technology Itd.L-75-1, and thickness is about 1mm, presses cover glass then, uses 60mW/cm again
2High voltage mercury lamp radiation 10～20s after ultra-violet curing glue promptly solidify, so far finish encapsulation process.
TEOLED device cut-in voltage is V before the encapsulation
0=3.2～3.3V, I
0=0.00281mA; After the encapsulation, measuring cut-in voltage again is V
0=4.2～4.3V, I
0=0.00327mA.
Encapsulation is preceding at V
1=7 o'clock, measuring its brightness was 4696cd/m
2, after the encapsulation through 20 days, at V
1=7 times, surveying its brightness is 4588cd/m
2, illustrate that packaging effect is good.
Embodiment 2:
Preparation of devices is carried out in multi-source organic molecule gas-phase deposition system, and detailed preparation process is as follows:
[1] silicon substrate is cleaned repeatedly with acetone, ethanol, deionized water successively and is ultrasonic, oven dry then;
[2] substrate of handling well is placed multi-source organic molecule gas-phase deposition system, comprise organic evaporating area (8 evaporation sources) and evaporation of metal district (2 evaporation sources) in the same vacuum cavity of system, completely cut off mutually between two districts and between each evaporation source, avoided mutual pollution, substrate can rotate to organic evaporating district or top, evaporation of metal district respectively, make things convenient for the growth of material, substrate distance evaporation source 25cm, can rotation and revolution to guarantee the uniformity of metal film and organic membrane, material therefor is placed on respectively in the different evaporation sources of different evaporating area, the temperature of each evaporation source can be controlled separately, is evacuated to 3 * 10 then
-4Pa;
[3] under above-mentioned vacuum condition, the Ag that evaporation 70nm is thick on substrate earlier is as anode, again successively evaporation 45nm thick 4,4 ', 4 "-three (3-aminomethyl phenyl aniline) triphenylamine (m-MTDATA) is as hole injection layer; the N that 5nm is thick; N '-two-(1-phenyl)-N, N '-diphenyl-1,1 '-xenyl-4; 4 '-diamines (NPB) is as hole transmission layer, three (oxine) aluminium (Alq that 60nm is thick
3) as luminescent layer and electron transfer layer, the thick LiF of 1nm is as electron injecting layer, the thick Ag of last Al that evaporation 1nm is thick again and 22nm is as semitransparent cathode.
[4] again with substrate-transfer to the organic evaporating district, it is constant to keep above-mentioned vacuum condition, evaporation ZnS on negative electrode, the speed of growth is 0.1nm/s, thickness is 50nm.
The thickness of the above material growth and growth rate are produced the control of L-400 film-thickness monitoring by the U.S., and the device performance of preparation gained is tested under the normal temperature condition in air with PR650 spectrometer and Keithley2400 current/voltage source.
Grown behind the ZnS film, device is put into the Braun glove box, be coated with last layer ultra-violet curing glue in the luminous zone of device earlier, thickness is about 1mm, presses cover glass then, uses 60mW/cm again
2High voltage mercury lamp radiation 10～20s after ultra-violet curing glue promptly solidify, so far finish encapsulation process.TEOLED device cut-in voltage is V before the encapsulation
0=3.0～3.1V, I
0=0.00301mA; After the encapsulation, measuring cut-in voltage again is V
0=3.8～4.0V, I
0=0.00596mA.
Encapsulation is preceding at V
1During=7V, measuring its brightness is 5537cd/m
2, after the encapsulation through 20 days, at V
1During=7V, surveying its brightness is 5389cd/m
2, illustrate that packaging effect is good.
Embodiment 3:
Preparation of devices is carried out in multi-source organic molecule gas-phase deposition system, and detailed preparation process is as follows:
[1] silicon substrate is cleaned repeatedly with acetone, ethanol, deionized water successively and is ultrasonic, oven dry then;
[2] substrate of handling well is placed multi-source organic molecule gas-phase deposition system, comprise organic evaporating area (8 evaporation sources) and evaporation of metal district (2 evaporation sources) in the same vacuum cavity of system, completely cut off mutually between two districts and between each evaporation source, avoided mutual pollution, substrate can rotate to organic evaporating district or top, evaporation of metal district respectively, make things convenient for the growth of material, substrate distance evaporation source 25cm, can rotation and revolution to guarantee the uniformity of metal film and organic membrane, material therefor is placed on respectively in the different evaporation sources of different evaporating area, the temperature of each evaporation source can be controlled separately, is evacuated to 3 * 10 then
-4Pa;
[3] under above-mentioned vacuum condition, the Ag that evaporation 70nm is thick on substrate earlier is as anode, again successively evaporation 45nm thick 4,4 ', 4 "-three (3-aminomethyl phenyl aniline) triphenylamine (m-MTDATA) is as hole injection layer; the N that 5nm is thick; N '-two-(1-phenyl)-N, N '-diphenyl-1,1 '-xenyl-4; 4 '-diamines (NPB) is as hole transmission layer, three (oxine) aluminium (Alq that 60nm is thick
3) as luminescent layer and electron transfer layer, the thick LiF of 1nm is as electron injecting layer, the thick Ag of last Al that evaporation 1nm is thick again and 22nm is as semitransparent cathode.
[4] again with substrate-transfer to the organic evaporating district, it is constant to keep above-mentioned vacuum condition, evaporating Al q on negative electrode
3, the speed of growth is 0.1nm/s, thickness is 78nm.
The thickness of the above material growth and growth rate are produced the control of L-400 film-thickness monitoring by the U.S., and the device performance of preparation gained is tested under the normal temperature condition in air with PR650 spectrometer and Keithley2400 current/voltage source.
Alq has grown
3Behind the film, device is put into the Braun glove box, be coated with last layer ultra-violet curing glue in the luminous zone of device earlier, thickness is about 1mm, presses cover glass then, uses 60mW/cm again
2High voltage mercury lamp radiation 10～20s after ultra-violet curing glue promptly solidify, so far finish encapsulation process.TEOLED device cut-in voltage is V before the encapsulation
0=3.0～3.1V, I
0=0.00291mA; After the encapsulation, measuring cut-in voltage again is V
0=3.7～3.8V, I
0=0.00306mA.
Encapsulation is preceding at V
1During=7V, measuring its brightness is 5637cd/m
2, after the encapsulation through 20 days, at V
1During=7V, surveying its brightness is 5560cd/m
2, illustrate that packaging effect is good.
Embodiment 4:
Preparation of devices is carried out in multi-source organic molecule gas-phase deposition system, and detailed preparation process is as follows:
[1] silicon substrate is cleaned repeatedly with acetone, ethanol, deionized water successively and is ultrasonic, oven dry then;
[2] substrate of handling well is placed multi-source organic molecule gas-phase deposition system, comprise organic evaporating area (8 evaporation sources) and evaporation of metal district (2 evaporation sources) in the same vacuum cavity of system, completely cut off mutually between two districts and between each evaporation source, avoided mutual pollution, substrate can rotate to organic evaporating district or top, evaporation of metal district respectively, make things convenient for the growth of material, substrate distance evaporation source 25cm, can rotation and revolution to guarantee the uniformity of metal film and organic membrane, material therefor is placed on respectively in the different evaporation sources of different evaporating area, the temperature of each evaporation source can be controlled separately, is evacuated to 3 * 10 then
-4Pa;
[3] under above-mentioned vacuum condition, the Al that earlier evaporation 45nm is thick on substrate is as negative electrode, and the LiF of evaporation 1nm is as electron injecting layer again, three (oxine) aluminium (Alq that 60nm is thick
3) as luminescent layer and electron transfer layer, the N that 5nm is thick, N '-two-(1-phenyl)-N, N '-diphenyl-1,1 '-xenyl-4,4 '-diamines (NPB) is as hole transmission layer, 45nm thick 4,4 ', 4 "-three (3-aminomethyl phenyl aniline) triphenylamine (m-MTDATA) is as hole injection layer, and the Ag of last evaporation 22nm is as translucent anode.
[4] again with substrate-transfer to the organic evaporating district, it is constant to keep above-mentioned vacuum condition, evaporation ZnO on anode, the speed of growth is 0.1nm/s, thickness is 60nm.
The thickness of the above material growth and growth rate are produced the control of L-400 film-thickness monitoring by the U.S., and the device performance of preparation gained is tested under the normal temperature condition in air with PR650 spectrometer and Keithley2400 current/voltage source.
Grown behind the ZnO film, device is put into the Braun glove box, be coated with last layer ultra-violet curing glue in the luminous zone of device earlier, thickness is about 1mm, presses cover glass then, uses 60mW/cm again
2High voltage mercury lamp radiation 10～20s after ultra-violet curing glue promptly solidify, so far finish encapsulation process.TEOLED device cut-in voltage is V before the encapsulation
0=3.1～3.2V, I
0=0.00271mA; After the encapsulation, measuring cut-in voltage again is V
0=3.9～4.0V, I
0=0.00294mA.
Encapsulation is preceding at V
1During=7V, measuring its brightness is 5496cd/m
2, after the encapsulation through 20 days, at V
1During=7V, surveying its brightness is 5406cd/m
2, illustrate that packaging effect is good.
The above only is the specific embodiment of the present invention, can not limit scope of the invention process with it, and the impartial changes and improvements of carrying out according to patent claim of the present invention all should still belong to the scope that patent of the present invention contains generally.
Claims (10)
1, a kind of method for packing of top radiation organic EL part, it comprises the steps:
A. make the organic electroluminescence device of top emission;
B. on the top electrode of device evaporation one deck at visible region transmitance more than 70%, the easily organic material or the inorganic material protective layer of evaporation;
C. on protective layer, apply ultra-violet curing glue;
D. the transparent enclosure cover plate is pressed onto on the ultra-violet curing glue;
E. the ultraviolet irradiation device makes the ultra-violet curing adhesive curing, finishes the encapsulation to device.
2, the method for packing of a kind of top radiation organic EL part as claimed in claim 1 is characterized in that: top radiation organic EL part is the top ballistic device of positive interposed structure.
3, the method for packing of a kind of top radiation organic EL part as claimed in claim 2 is characterized in that: the structure of the top ballistic device of positive interposed structure is substrate/anode/hole injection layer/hole transmission layer/luminescent layer/electron transfer layer/electron injecting layer/negative electrode top electrode.
4, the method for packing of a kind of top radiation organic EL part as claimed in claim 1 is characterized in that: top radiation organic EL part is the top ballistic device of inverted structure.
5, the method for packing of a kind of top radiation organic EL part as claimed in claim 4 is characterized in that: the structure of the top ballistic device of inverted structure is substrate/negative electrode/electron injecting layer/electron transfer layer/luminescent layer/hole transmission layer/hole injection layer/anode top electrode.
6, the method for packing of a kind of top radiation organic EL part as claimed in claim 1; it is characterized in that: the organic material protective layer of evaporation is 4; 4 '-N, N-two carbazoles-biphenyl, three (oxine) aluminium, N, N '-two-(1-phenyl)-N; N '-diphenyl-1; 1 '-xenyl-4,4 '-diamines or 2,9-dimethyl-4; 7-diphenyl-1,10-joins phenanthroline.
7, the method for packing of a kind of top radiation organic EL part as claimed in claim 1 is characterized in that: the inorganic material protective layer of evaporation is MoO
3, WO
3, ReO
3, ZnO, TeO
2, ZnS or ZnSe
8, the method for packing of a kind of top radiation organic EL part as claimed in claim 1 is characterized in that: the transparent enclosure cover plate is simple glass sheet, polymethyl methacrylate sheet or colored filter.
9, as the method for packing of any one described a kind of top radiation organic EL part of claim 1～8, it is characterized in that: the thickness of protective layer is 10nm～100nm.
10, the application of the method for packing of any one described a kind of top radiation organic EL part of claim 1～8 aspect the packaging electronic electric device.
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2008
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