CN100496174C - Method for preparing film from material and its organic electroluminescent device - Google Patents

Method for preparing film from material and its organic electroluminescent device Download PDF

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CN100496174C
CN100496174C CNB2005100804738A CN200510080473A CN100496174C CN 100496174 C CN100496174 C CN 100496174C CN B2005100804738 A CNB2005100804738 A CN B2005100804738A CN 200510080473 A CN200510080473 A CN 200510080473A CN 100496174 C CN100496174 C CN 100496174C
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evaporation
film
preparation
alq
source
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CN1725913A (en
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邱勇
张德强
张祝新
高裕弟
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Tsinghua University
Beijing Visionox Technology Co Ltd
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Tsinghua University
Beijing Visionox Technology Co Ltd
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Abstract

A method for preparing material to be film uses multiple evaporation source to evaporate one material and with different evaporation rates of multiple evaporation sources. An organic electro-fluorescence component has at least one material being prepared by multiple source evaporation. The method can form film in high rate and the prepared organic electro- fluorescence component applies low voltage and high brightness and long service time.

Description

The method of preparing film forming of material and organic electroluminescence device thereof
Technical field
The present invention relates to a kind of film build method of material, relate in particular to the film build method of material in the organic electroluminescence device and the organic electroluminescence device made of method thus.
Background technology
Be the film forming speed of material in the faster devices, take to improve the method that film-forming temperature improves the deposition rate of material usually.But material is generally along with the raising of temperature, and the particle diameter of the material that is evaporated can become greatly, thereby has reduced the compactness and the continuity of film.And when the evaporation temperature was too high, the stability of material hydatogenesis also can descend, and when temperature was too high, material can intermittently spray evaporation source.
When evaporation under a certain fixed temperature, the granular size of material is often close in the rete, but from forming on the more fine and close rete angle, is made of the rete that the fine and close continuity of easier formation is high in the rete the alternate particle of granular size.
And in fields such as organic electroluminescents, very high to the compactness and the successional requirement of various functional layer film in the device, the defective of functional layer film can be brought not problems such as bright spot, short circuit in the device, and device performance is low.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of method and organic electroluminescence device prepared by this method of the fine and close continuous films of formation of high speed.
Technical scheme of the present invention is: a kind of film build method of material, carry out evaporation to commaterial simultaneously with a plurality of evaporation sources.
The evaporation speed of a plurality of evaporation sources can be different.
A kind of organic electroluminescence device, at least a material is to make with the film build method of multi-source evaporation in this device.Adopting the material of said method evaporation can be hole mobile material, can be N, N '-two-(1-naphthyl)-N, and N '-diphenyl-1,1-xenyl-4, the 4-diamines also can be the luminescent layer material, can be oxine aluminium.
The invention has the beneficial effects as follows: under the constant situation of the film-forming temperature of material, method by a plurality of evaporation source common deposited is come film forming, total rate of film build is the summation of each evaporation source deposition rate, under the prerequisite that does not influence film quality, improve film forming speed, thereby under the prerequisite that does not influence device performance, improved the production efficiency of device.And the evaporation speed of at least two evaporation sources in a plurality of evaporation sources is not simultaneously, forms the film layer structure that the granularity size is intersected easily, obtains finer and close continuous rete like this, and device performance is better.
Description of drawings
1, the AFM of embodiment 1 figure.
2, the AFM of embodiment 2 figure.
3, the AFM of Comparative Examples 1 figure.
4, the AFM of embodiment 5 figure.
5, the AFM of Comparative Examples 3 figure.
Embodiment
Term " a plurality of evaporation source " is meant two or more evaporation sources.Oxine aluminium abbreviates AlQ as,
Structural formula is
Figure C200510080473D00041
N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4, the 4-diamines abbreviates NPB as, structural formula
For:
Figure C200510080473D00042
Embodiment 1: double source is with the preparation of fast AlQ rete
1, the preparation of AlQ material and evaporation source: the AlQ material of identical weight is packed in two identical crucibles, put into the different evaporation sources of same vacuum chamber, be evacuated down to 1.6 * 10 -4Pa.
2, double source is with the preparation of fast AlQ rete: the silicon chip of cleaning, drying surfacing is placed in the vacuum chamber, and be delivered in the chamber that the AlQ material is housed, be evacuated down to 1.6 * 10 -4Pa, regulate the deposition rate of the AlQ material in two evaporation sources, make the deposition rate of AlQ material of two evaporation sources basic identical, all be 0.25nm/s, begin deposition, observe the thickness indication of the film thickness detector of two AlQ evaporation sources, when the thickness of two AlQ evaporation sources all reaches 60nm, stop deposition simultaneously.
The preparation of the different fast AlQ retes of embodiment 2 double sources:
Preparation technology is with embodiment 1, and difference is that in the evaporate process, the evaporation speed of control double source is respectively 0.4nm/s and 0.1nm/s.
The preparation of Comparative Examples 1 single source high speed AlQ rete:
Adopt traditional single source to prepare the AlQ film, single source evaporation rate controlled is 0.5nm/s, and other film preparation conditions are with embodiment 1 and 2.
Observe AFM (atomic force microscope) pattern of the AlQ rete for preparing under the different condition: the substrate glass of AlQ film that will be by above method preparation is taken out from vacuum chamber, carries out mark, uses AFM scanning surface topography respectively, and the result is as follows:
Figure C200510080473D00043
Can see by accompanying drawing 1-3 and top data, under identical higher total evaporation speed 0.5nm/s, the more smooth densification of film when adopting two evaporation sources the film during evaporating Al Q adopting single evaporation source simultaneously is continuous, and when adopting the different speed evaporation of two evaporation sources, the granular size that forms is alternate, and the film of formation is finer and close continuously.
Utilize three kinds of conditions further to prepare the device of same structure, and its performance is contrasted, device architecture is: ITO/NPB (50nm)/AlQ (50nm)/LiF/Al, and preparation process is respectively:
Embodiment 3: double source is with fast AlQ preparation of devices
1, be carved with the cleaning of the glass substrate of ITO figure in advance: the washing agent of utilization heat is ultrasonic to be cleaned the glass substrate that is carved with the ITO figure in advance with the ultrasonic method of deionized water, cleans the back and dries in cleaning oven.
2, import substrate into vacuum chamber, be evacuated to 1.6 * 10 -4Pa.
3, deposition one deck hole mobile material NPB on ito substrate, deposition rate is 0.2nm/s, thickness is 50nm.
4, adopt the film build method deposition one deck luminous organic material AlQ of double source with speed again on hole mobile material NPB, the thickness of AlQ is 60nm, and the deposition rate of double source AlQ is 0.25nm/s.
5, the preparation of LiF layer: substrate is delivered to the chamber for preparing metallic cathode, is evacuated down to 1.6 * 10 -4Pa, deposition one deck LiF on the AlQ layer, thickness 0.7nm, deposition rate 0.01nm/s.
6, the preparation of negative electrode: keep above-mentioned vacuum chamber internal pressure constant, deposition AL film is as cathode material on the LiF layer, and the thickness of AL film is 150nm, and deposition rate is 1.5nm/s.
7, the device after the preparation adopts UV to solidify the glue encapsulation.
Embodiment 4: the different fast AlQ preparation of devices of double source:
Preparation technology is with embodiment 3, and difference is that in the evaporate process, the evaporation speed of control double source is respectively 0.4nm/s and 0.1nm/s.
Comparative Examples 2 single source high speed AlQ preparation of devices:
Preparation technology is with embodiment 3, and difference is that in the evaporate process, the AlQ layer film adopts the method preparation of single source evaporation, and preparation speed is 0.5nm/s.
The performance comparison result of device is as follows:
Figure C200510080473D00051
Find by contrast: evaporating Al Q under identical higher evaporation speed, the device of the method for the more single source of the method high speed evaporation of employing double source evaporation is because the film that forms is finer and close continuously, and the performances such as bright voltage, efficient, brightness, life-span that open of device are improved.When two evaporation sources adopted different evaporation speed, device performance further improved.
Embodiment 5: double source is with the preparation of fast NPB film
1.NPB the preparation of material and evaporation source: the NPB material of identical weight is packed in two identical crucibles, put into the different evaporation sources of same vacuum chamber, be evacuated down to 1.6 * 10 -4Pa.
2. double source is with the preparation of fast NPB rete: the silicon chip of cleaning, drying surfacing is placed in the vacuum chamber, and be delivered in the chamber that the NPB material is housed, be evacuated down to 1.6 * 10 -4Pa, regulate the deposition rate of the NPB material in two evaporation sources, make the deposition rate of NPB material of two evaporation sources basic identical, all be 0.20nm/s, begin deposition, observe the thickness indication of the film thickness detector of two NPB evaporation sources, when the thickness of two NPB evaporation sources all reaches 60nm, stop deposition simultaneously.
Comparative Examples 3: the preparation of the different fast NPB films of double source
Employing is carried out the preparation of NPB film with embodiment 5 identical conditions, and difference is that in this preparation process the evaporation rate controlled of NPB double source is 0.3nm and 0.1nm.
Figure C200510080473D00061
Can see by accompanying drawing 4-5 and top data, double source evaporation under identical higher total evaporation speed 0.4nm/s, when the different speed evaporation of two evaporation sources, the film of formation is finer and close continuously.
Embodiment 6: double source is with fast NPB preparation of devices
1. be carved with the cleaning of the glass substrate of ITO figure in advance: the washing agent of utilization heat is ultrasonic to be cleaned the glass substrate that is carved with the ITO figure in advance with the ultrasonic method of deionized water, cleans the back and dries in cleaning oven.
2. import substrate into vacuum chamber, be evacuated to 1.6 * 10 -4Pa.
3. adopt the method deposition one deck hole mobile material NPB with step 2 on ito substrate, thickness is 60nm.
4. deposit one deck luminous organic material AlQ on hole mobile material NPB again, the thickness of AlQ is 50nm, and deposition rate is 0.2nm/s.
5.LiF the preparation of layer: substrate is delivered to the chamber for preparing metallic cathode, is evacuated down to 1.6 * 10 -4Pa, deposition one deck LiF on the AlQ layer, thickness 0.7nm, deposition rate 0.01nm/s.
6. the preparation of negative electrode: keep above-mentioned vacuum chamber internal pressure constant, deposition AL film is as cathode material on the LiF layer, and the thickness of AL film is 150nm, and deposition rate is 1.5nm/s.
7. the device after the preparation adopts UV to solidify the glue encapsulation.
Comparative Examples 4: the different fast NPB preparation of devices of double source
Employing is carried out preparation of devices with embodiment 6 identical conditions, and difference is that in this preparation process the evaporation rate controlled of NPB double source is 0.3nm and 0.1nm.
The morphology analysis of film and device performance contrast are as follows:
Find by contrast: double source evaporation NPB under identical higher evaporation speed, the asynchronous device of the speed of two evaporation sources is because the film that forms is finer and close continuously, and the performances such as bright voltage, efficient, brightness, life-span that open of device are improved.When two evaporation sources adopted different evaporation speed, device performance further improved.
Do not want to be subject to the theory how the present invention realizes, can belong to the combination of various factors to the raising of electroluminescent properties in the organic electroluminescence device in of the present invention.For example, the difference of speed also may influence the crystallization degree of material, influences the carrier mobility of device, finally influences device performance.

Claims (6)

1, a kind of method with preparing film forming of material is characterized in that simultaneously commaterial being carried out evaporation with a plurality of evaporation sources.
2, the film build method of material as claimed in claim 1 is characterized in that the evaporation speed difference at least two sources in a plurality of evaporation sources.
3, a kind of organic electroluminescence device is characterized in that at least a material in the device is to prepare film forming with claim 1 or 2 described methods.
4, organic electroluminescence device as claimed in claim 3 is characterized in that described at least a material is a kind of material in the hole transmission layer.
5, organic electroluminescence device as claimed in claim 4 is characterized in that a kind of material in the described hole transmission layer is N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4,4-diamines.6, organic electroluminescence device as claimed in claim 3 is characterized in that described at least a material is a kind of material in the luminescent layer.
7, organic electroluminescence device as claimed in claim 6 is characterized in that a kind of material in the described luminescent layer is an oxine aluminium.
CNB2005100804738A 2005-02-04 2005-07-05 Method for preparing film from material and its organic electroluminescent device Active CN100496174C (en)

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