CN100440578C - manufacturing method for organic EL element - Google Patents
manufacturing method for organic EL element Download PDFInfo
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- CN100440578C CN100440578C CNB031368778A CN03136877A CN100440578C CN 100440578 C CN100440578 C CN 100440578C CN B031368778 A CNB031368778 A CN B031368778A CN 03136877 A CN03136877 A CN 03136877A CN 100440578 C CN100440578 C CN 100440578C
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- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09G—ARRANGEMENTS OR CIRCUITS FOR CONTROL OF INDICATING DEVICES USING STATIC MEANS TO PRESENT VARIABLE INFORMATION
- G09G3/00—Control arrangements or circuits, of interest only in connection with visual indicators other than cathode-ray tubes
- G09G3/006—Electronic inspection or testing of displays and display drivers, e.g. of LED or LCD displays
Abstract
To provide a manufacturing method of an EL element capable of previously properly opening and breaking a film defective part without damaging a normal part of the element. This manufacturing method of an EL element comprises a process for forming the organic EL element with an organic film interposed between a positive electrode and a negative electrode, and an aging process for opening and breaking the defective part in an aging process for applying a voltage between the positive electrode and the negative electrode in the organic EL element. The puncture voltage of the defective part and the puncture voltage of the organic EL element are found by measuring the current when applying a reverse bias voltage to the organic EL element, and thereafter the aging is executed by using a voltage range between both puncture voltages for the range of the application voltage in the aging. (C)2004,JPO.
Description
Technical field
The present invention relates to be used for the manufacture method of organic EL (electroluminescence) element of display etc., relate in particular to aging method as the stabilization processes method that improves the display qualification rate.
Prior art
EL element is because oneself is luminous, thereby the visibility height, is complete solid-state components, has the feature of excellent impact resistance, thus adopted the various elements of inorganic compound and organic compound to be suggested at present, and drop into practical probation.
The organic membrane that organic EL in these elements wrapped folder between anode and negative electrode comprises luminous organic material forms.This organic EL is owing to can adopt the low voltage drive of number V～ten number V, thereby it is low to consume electric power, can comprise drive circuit and realize lightweight, various application such as the thin display of future generation of the present widely used LCD of replacement that therefore waits in expectation and flat illumination, slim back side light.
Yet organic EL exists interelectrode organic membrane (such as submicron order) as thin as a wafer, even the defective part that takes place in this electrode film and the organic membrane (film defective part) is small, electric current is also concentrated easily, causes non-luminous problem.
As the reason of this tiny flaw, can enumerate the dust that when forming the film of electrode and so-called organic membrane, is taken place and consider grain etc. to be worth doing, but will on large tracts of land, not produce these defectives, the film that forms homogeneous is very difficult.
Therefore, consider in element manufacturing process, to carry out between anode and negative electrode, applying the burin-in process of voltage, make the film defective part destruction of opening a way in advance.So-called open circuit destroys and means and make the defective part non-conductorization, by destroy the electrode corresponding with this film defective part by the Joule heat that is produced when aging, becomes open-circuit condition (state of insulation), or oxidation and form phenomenon such as non-conductorization and take place.
Become local non-illuminating part though carried out the film defective part of this open circuit destruction, the film defective part that becomes problem can not be looked small the part of recognizing originally exactly, to not influence of display quality, does not become problem.
As the technology of carrying out based on the open circuit destruction of this burin-in process, open in the clear 61-114493 communique the spy, the aging method in a kind of inorganic EL element has been proposed.The method is characterized in that, apply direct voltage, make the film defective part that exists in the element produce small destruction,, apply alternating voltage then as the 2nd aging process as the 1st aging process.
But, though this aging method is an effective method,, the anxiety of the organic EL of destruction own is arranged then in the inorganic EL element of electroluminescence type if adopt same quadrat method for galvanoluminescence type organic EL.That is, even the normal portion that does not have the film defective part in the element also may damage owing to interelectrode short circuit and based on this disappearance etc. of organic membrane.
In No. 2818255 specification of this external patent, following method has been proposed: to organic EL, as the 1st aging process, with 1 * 10
4～1 * 10
7Voltage in the V/cm scope applies successively respectively more than 1 second that the direct current para-electric is pressed and direct current back voltage more than 1 second, carries out burin-in process, then as the 2nd aging process, applies the direct current para-electric pressure that its time is longer than the 1st aging process.
Though in the method, among the embodiment in above-mentioned specification in the past, become the index of the stabilized driving of element based on the reduction of the current value of the back voltage of aging process, but there is query in qualitative going up on the reliability this point, this aging method is also same with the aging method of above-mentioned communique in the past simultaneously, do not implement if do not consider the voltage endurance of organic EL, then may destroy element itself.
Organic EL at (between anode and the negative electrode) lamination multilayer organic membrane between upper/lower electrode, is generally 5 layers to 7 layers usually, and is complicated.The material of these multilayer films and thickness are also in response to various differences are arranged with object in addition.Therefore aging method in the past is not that all component structures generally are suitable for.
That is, the different various organic ELs of this layer structure generally are suitable for, can realize the open circuit destruction of film defective part reliably simultaneously and prevent that the aging method of the destruction of normal portion from being non-existent in the past.
Summary of the invention
The present invention its objective is that providing a kind of does not cause damage to the normal portion of element in view of the above problems, and makes the film defective part method for manufacturing organic EL destroyed of open circuit suitably in advance.
That is, in the present invention, a kind of method for manufacturing organic EL, it possesses the operation that is formed on the organic EL S1 that wrapped folder organic membrane 3～6 forms between anode 2 and the negative electrode 8;
In above-mentioned organic EL, carry out between above-mentioned anode and above-mentioned negative electrode, applying the burin-in process of voltage, make the aging process of the defective part open circuit destruction that exists in the film,
It is characterized in that:
After the electric current that flows when having applied anti-bias voltage by being determined in the above-mentioned organic EL, the open circuit of having obtained above-mentioned defective part destroy the voltage range that takes place and above-mentioned organic EL and produce the voltage range of destroying,
The open circuit of this defective part destroyed minimum voltage and organic EL in the voltage range that takes place produces the voltage range between the minimum voltage in the voltage range of destroying and the voltage range more than the back voltage absolute value when being the actual driving of above-mentioned organic EL, as the scope that applies voltage in the above-mentioned burin-in process, carry out above-mentioned aging process.。
Like this,, carry out in the voltage range of burin-in process between these two disintegration voltages, thereby can not destroy normal portion, the defective part open circuit is destroyed owing to obtain the disintegration voltage of defective part and the disintegration voltage of organic EL in advance.
Here can consider that organic EL has diode characteristic, under anti-bias voltage,, reach open circuit by Joule heat defective part and destroy based on this leakage current at defective part generation leakage current.As mentioned above, though the ruinate defective part of opening a way becomes local non-luminous point, owing to naked eyes can not be found, thereby to not influence of display quality.
Therefore,, can provide a kind of and can be not the normal portion of element not caused damage, and make the defective part method for manufacturing organic EL destroyed of open circuit suitably in advance according to the present invention.
For making defective part, preferably organic EL (S1) has been carried out after the heat treated in addition, or in heat treated, carried out aging process than more obviousization of room temperature state.
According to present inventor's etc. discussion, defective part is in the condition of high temperature more than room temperature state and becomes obvious more.That is,, can find to have the defective part of the possibility that timeliness takes place reliably by becoming the condition of high temperature.
That is,,, defective part is obviously changed than room temperature state, then can this defective part of obviously having changed open circuit be destroyed by aging process if organic EL is carried out heat treated according to the present invention.Therefore, can make have the possibility that timeliness takes place defective part in advance reliably open circuit destroy.
The structural material of organic membrane (3～6) is at least a preferably by the vacuum vapour deposition film forming in addition, the material that has vapo(u)rability when its film forming.
In organic EL, the organic membrane structure material is multiple by having of vacuum vapour deposition film forming, can roughly be divided into when its film forming the vapo(u)rability material that gasifies via liquid from solid and from the sublimability material of solid direct gasification.
According to present inventor's etc. discussion,, thereby more easily produce the space because wherein sublimability material one side is interparticle less in conjunction with energy.Therefore, be tending towards the high temperature space more and just become big more, the electrical leak between electrodes stream in the element also increases simultaneously.Infer that thus this space is the reason of defective part.
Therefore, preferably pass through at least a employing vapo(u)rability material of the structural material of organic membrane, reduce above-mentioned space, consequently can reduce the generation of defective part.
And aging process is preferably in organic EL (S1) is placed on oxygen concentration is to carry out under the state in the atmosphere more than 1%.This is for making the defective part oxidation by aging, realize the required desirable atmosphere of non-conductorization, and according to present inventor's etc. discussion, oxygen concentration is being difficult to realize reliable non-conductorization below 1%.
In addition, possessing under the occasion that the element sealing process that organic EL (S1) is sealed by inclosure gas is arranged, be preferably in and implement aging process before the element sealing process, and the oxygen concentration of the inclosure gas that uses in the element sealing process is in below the oxygen concentration in the aging process.Like this, burin-in process can be implemented well, and the manufacturing of the organic EL of dark space generation can be realized suppressing.
Description of drawings
Fig. 1 is the broad cross-section map of the organic EL that relates to of embodiment of the present invention 1.
Fig. 2 is the process flow chart of the method for manufacturing organic EL that relates to of the above-mentioned execution mode 1 of expression.
Fig. 3 A and Fig. 3 B are the accompanying drawings of measurement result one example of the disintegration voltage in normal portion of expression and the defective part.
Fig. 4 is the disintegration voltage and the accompanying drawing that destroys the relation that number takes place in normal portion of expression and the defective part.
Fig. 5 is the chart of the result of the test of turning on light continuously of the organic EL that produces of the manufacture method of expression by above-mentioned execution mode 1.
Fig. 6 is the chart of the result of the test of turning on light continuously of the organic EL of expression comparative example.
Fig. 7 is the result's of the expression relation of having investigated the oxygen concentration of aging atmosphere and failure rate a accompanying drawing.
Fig. 8 is the variation of expression as above-mentioned execution mode 1, the process flow chart of the method for manufacturing organic EL under the occasion of implementing aging process before the element sealing process.
The accompanying drawing of the standing time when Fig. 9 is the oxygen concentration of having represented to have changed inclosure gas and the relation of dark space size.
Figure 10 be thickness t (nm) and the organic EL of expression organic membrane disintegration voltage (V), destroy the accompanying drawing of the relation of electric field strength (MV/cm).
Figure 11 is the accompanying drawing of distribution of the destruction electric field strength of expression organic EL.
Figure 12 is illustrated in the organic EL that present inventor waits trial-production, before high temperature is placed under 120 ℃, 2hr condition and after the accompanying drawing of V-I characteristic.
Figure 13 A-13C is that summary is represented based on to Alq
3Film has carried out fractographic result's Alq
3The accompanying drawing of film section.
Figure 14 is the curve chart of the temperature dependency of expression depth of interstices (D) shown in Figure 13.
Figure 15 is the process flow chart of the method for manufacturing organic EL that relates to of expression embodiment of the present invention 3.
Figure 16 is the chart of the result of the test of turning on light continuously of the organic EL that produces of the manufacture method of expression by above-mentioned execution mode 3.
Figure 17 is the process flow chart of the method for manufacturing organic EL variation that relates to of the above-mentioned execution mode 3 of expression.
Figure 18 is the process flow chart of the method for manufacturing organic EL that relates to of expression embodiment of the present invention 4.
Figure 19 is the chart of the leakage current density of the expression organic EL that is judged to be defective products by aging good the judgement.
Execution mode
(execution mode 1)
Fig. 1 is the accompanying drawing of the summary section structure of the organic EL S1 that relates to of expression embodiment of the present invention 1.Organic EL S1 shown in Figure 1 represents 1 pixel of display floater, and this display floater has such as the structure with a plurality of this element S1 planar configuration, promptly a plurality of dot structures.
In Fig. 1, on the one side as the glass substrate 1 of substrate, lamination has anode 2, hole injection layer 3, hole transporting layer 4, luminescent layer 5, electron supplying layer 6, electron injecting layer 7 and negative electrode 8 each film successively.
A structure example of each layer of expression anode 2～negative electrode 8.Anode 2 is by the ITO (oxide of indium and tin, indium tin oxide) film of the thickness 140nm of Zu Chenging, the film of the thickness 60nm that the film of the thickness 50nm that hole injection layer 3 is made up of CuPc (copper phthalocyanine complex), hole transporting layer 4 are made up of TPTE (four triphenylamines).
In this structure example, anode 2 forms the strip that extends along the mutually orthogonal direction with negative electrode 8 like this, and the intersection of two electrodes 2,8 constitutes as a pixel (illuminating part).That is,, have a plurality of dot structures with rectangular configuration as display floater.Such as, can form 256 * 64 dot structure.
Like this, in each pixel, by apply electric field between anode 2 and negative electrode 8, hole and electronics move to luminescent layer 5 in organic membrane 3～6, in luminescent layer 5 once more the coupling the result be in luminescent layer 5, carry out luminous.
Next, the manufacture method of this organic EL S1 is done to record and narrate.Fig. 2 is the process flow chart of the organic EL manufacture method that relates to of present embodiment 1.At first, on glass substrate 1, make anode 2 film forming and form pattern (formation anode), implement the surface treatment of the plasma that mixes with oxygen based on argon etc. by sputtering method etc.
On this basis, make above-mentioned organic membrane 3～6 film forming and form pattern (formation organic membrane) successively, next, make electron injecting layer 7, negative electrode 8 film forming and form pattern (formation negative electrode) successively by vapour deposition method etc.Form organic EL S1 thus.
Though do not add diagram, on glass substrate 1, seal members such as stainless cylinder of steel and cloche are set according to the principle that covers this organic EL S1, by inclosure gases such as drying nitrogens organic EL S1 is sealed (element sealing) thus.By above-mentioned operation, make a plurality of display floaters that constitute by organic EL S1.
Next, utilize an one in a plurality of display floaters that produce, the electric current that has flowed when having applied anti-bias voltage by being determined among the organic EL S1 is obtained the disintegration voltage of defective part and the disintegration voltage (disintegration voltage mensuration operation) of organic EL (normal portion).
This disintegration voltage is measured operation specifically, in the display floater of the above-mentioned configuration example that has formed 256 * 64 pixels (element S1), with 1 pixel is that an element S1 is as 1 sample, between the electrode 2,8 of element S1, with anode 2 as negative pole, with negative electrode 8 as anodal, from 0～-60V applies anti-bias voltage successively.Utilize parameter analyzer that the electric current that flows between the electrode 2,8 is at this moment measured.
The pixel (element) that has defective part and the pixel (element) of non-existent normal portion are carried out this mensuration.With the naked eye can not see in practice owing to defective part in addition, thereby confirm its existence, seen defective part and normal portion clearly by microscope.Fig. 3 represents this measurement result one example.
In Fig. 3, (a) and (b) be respectively in expression normal portion and the defective part separately anti-bias voltage (V) and between electrode 2,8 mobile current density (mA/cm
2) the accompanying drawing of relation.
Shown in Fig. 3 (a), in normal portion, after beginning to increase anti-bias voltage from 0V, sharply increase at-electric current that 47V degree (voltage of arrow IIIA among the figure) flows between electrode 2,8, the short circuit between the generating electrodes 2,8 is the destruction of normal portion.Promptly in this embodiment, the disintegration voltage of normal portion is that the disintegration voltage of organic EL is-the 47V degree.
On the other hand, shown in Fig. 3 (b), in defective part, after beginning to increase anti-bias voltage from 0V, the leakage current under-7V degree between the generating electrodes 2,8, the open circuit that defective part takes place down in-12V degree (voltage of arrow IIIB among the figure) destroys.Promptly in this embodiment, the disintegration voltage of defective part is-the 12V degree.
Apply along bias voltage if do not apply anti-bias voltage in addition, owing in normal portion, having more electric current to flow more than the defective part, thereby be difficult to monitor the destruction of defective part shown in Figure 3.Therefore this disintegration voltage is measured and is adopted anti-bias voltage.
Like this, in the display floater that the organic EL S1 routine by this constitutes, a plurality of pixels (element) have been carried out same mensuration.Fig. 4 represents its result's a example.In Fig. 4, transverse axis is represented disintegration voltage (V), and number (the generation number of the defective part of destroyed or the normal portion of destroyed) takes place in longitudinal axis representative.
As can be seen from Figure 4, the electric current action when having applied anti-bias voltage in organic EL can clearly separate the defective part disintegration voltage and the disintegration voltage of organic EL (normal portion) own of the voltage that destroys as film defective part open circuit.Like this, if specific these two disintegration voltages wear out according to the condition of having only defective part to reach destruction, the defective part (film defective part) that exists in electrode and the organic membrane is opened a way in advance destroy (non-conductorization).
In the example of Fig. 4, if the disintegration voltage of defective part adopts the defective part open circuit to destroy the minimum voltage among the voltage range IVB that takes place then is-8V, if employing defective part open circuit destroys the maximum voltage among the voltage range IVB that takes place then is-16V.In addition from preventing the destruction this point of normal portion reliably, the disintegration voltage of organic EL (normal portion) adopt as the minimum voltage among the voltage range IVA-36V.In each means of this external present embodiment and each execution mode described later, the big or small benchmark of voltage and the magnitude relationship between the voltage determine by absolute value.
Carry out above-mentioned disintegration voltage and measured operation, and after having obtained the disintegration voltage of the disintegration voltage of defective part and organic EL, voltage range between these two disintegration voltages as the scope that applies voltage in the burin-in process, is carried out applying the burin-in process (aging process) of voltage between anode 2 and negative electrode 8 in organic EL S1.
By this aging process, make reaching of existing in each film 2～8 can not look the tiny flaw portion open circuit destruction of recognizing degree.In this aging process, owing to carry out burin-in process in the voltage range between the disintegration voltage of the disintegration voltage of defective part and organic EL, thereby normal portion can not destroy, and only makes defective part open circuit destruction.If visual defective part of recognizing exists in each film 2～8 in addition, before aging process, can easily remove.
As mentioned above, consider that organic EL has diode characteristic, under the anti-bias voltage of above-mentioned scope,, reach open circuit by Joule heat defective part and destroy based on this leakage current at defective part generation leakage current.Ruinate defective part becomes local non-luminous point though open a way, owing to naked eyes can not be found, thereby to not influence of display quality.Therefore, can provide a kind of and the normal portion of element not caused damage, and make the defective part method for manufacturing organic EL destroyed of open circuit suitably in advance.
Specifically, aging process carries out the panel beyond the display floater that provides in the disintegration voltage mensuration operation.Like this, behind aging process, to the test (turn on light check operation) etc. of turning on light of each panel, a shipping no problem panel on characteristic gets final product.
Based on the example of above-mentioned Fig. 4, aging process can with-8V to-16V above-voltage range between 36V is following implements as the voltage range that applies in the burin-in process.
In addition based on the example of Fig. 4, if as the disintegration voltage of defective part, adopt the open circuit of defective part to destroy minimum voltage-8V among the voltage range IVB that takes place ,-8V～-select the aging voltage that applies in the scope of 36V, then normal portion can not destroy, and the defective part open circuit is destroyed.
Yet, if as the disintegration voltage of defective part, adopt the open circuit of defective part to destroy maximum voltage-16V among the voltage range IVB that takes place ,-16V～-select the aging voltage that applies in the voltage range IV of 36V, a plurality of defective part open circuits are destroyed, thereby wish so.In addition in Fig. 4, with-16V～-the voltage range IV of 36V is as " destroy the defective part open circuit, and the non-destructive voltage range of element ".
Preferably the defective part open circuit being destroyed the minimum voltage and the organic EL S1 (normal portion) that take place in addition produces between the minimum voltage that destroys as the scope that applies voltage in the burin-in process.
This in the example of Fig. 4, with aging apply voltage and be set to-8V～-36V between.Like this, can realize more reliably that the normal portion that reaches of the open circuit destruction of defective part is preventing of organic EL destruction, wish so.
Also the defective part open circuit can be destroyed the minimum voltage and the defective part open circuit that take place in addition destroys between the maximum voltage that takes place as the scope that applies voltage in the burin-in process.
This in the example of Fig. 4, with aging apply voltage and be set to-8V～-16V between.Like this, can realize more reliably that also the normal portion that reaches of the open circuit destruction of defective part is preventing of organic EL destruction, wish so.
Effect to the aging process in the organic EL manufacture method of present embodiment 1 is explained based on a concrete example.In the concrete example of this effect, to having the display floater of above-mentioned 256 * 64 dot structures, the burin-in process of utilizing drive circuit to carry out 1 minute by the dry nitrogen atmosphere that contains 4% oxygen at room temperature.
In this concrete example, applying waveform is 125Hz, the rectangular pulse of 1/64 duty.The details in 1 cycle is, applies 1 time along bias voltage 12V, then applies anti-bias voltage-25V 63 times.
Here ,-anti-bias voltage of 25V is based on the voltage that applies in the burin-in process of the voltage range between the disintegration voltage of the disintegration voltage of defective part and organic EL.Therefore, by this anti-bias voltage defective part open circuit taking place destroys.By applying, can utilize the drive circuit of common organic EL to send the aging voltage that applies in addition along bias voltage.
Like this, to proceeding to the panel of aging process, implemented the test of turning on light continuously in 85 ℃ of thermostats.As a comparative example, to the element sealing process in the process flow chart that proceeds to Fig. 2, do not carry out the display floater of later aging process and test too.
Fig. 5 represents that (this result of the test of panel number A1～A5), Fig. 6 represents comparative example (this result of the test of panel number J1～J6) for the concrete example of present embodiment.Here, to each panel, at least 1 element in 256 * 64 elements, be the time that short circuit takes place between the electrode 2,8 to be made as capable defective time of origin with the row defective.
As shown in Figure 6, in comparative example, capable defective all taken place be the short circuit between the electrode 2,8 in 20 hours.Relative therewith, as shown in Figure 5, in the panel of the burin-in process of having implemented present embodiment, confirm the effect of time of origin prolongation more than 3 times of trip defective.
As mentioned above,, can provide a kind of and the normal portion of element not caused damage, and make the defective part method for manufacturing organic EL destroyed of open circuit suitably in advance according to present embodiment 1.
Like this, because the organic EL S1 that produces according to this manufacture method interelectrode short circuit in the defective part and leakage current after shipment be difficult to take place, can realize that therefore the deficiency of row defective etc. significantly reduces the organic EL that reliability is high.
Here, in above-mentioned aging concrete example, implement respectively along bias voltage apply, anti-bias voltage applies.Like this, can utilize the common drive circuit of organic EL to implement to wear out, especially not need aging special circuit, thereby be efficient.
Above-mentioned in addition aging process is preferably in organic EL S1 is placed under the state in the atmosphere of oxygen concentration more than 1% and carries out.This is because as described later, and the discussion according to present inventor etc. if oxygen concentration less than 1% will make the defective part oxidation owing to aging, is difficult to non-conductorization reliably.
Fig. 7 is the result's of the expression relation of having investigated the oxygen concentration of aging atmosphere and failure rate a accompanying drawing.Here, failure rate (%) expression will work as when 85 ℃ have been carried out driving in 1000 hours to the panel with a plurality of organic ELs, the time conduct that the row defective takes place in a pixel of panel at least the ratio of the fault panel during fault.Fail to take place owing to wearing out under the occasion of open circuit destruction and non-conductorization in defective part, this failure rate increases.
As shown in Figure 7, insufficient if oxygen concentration is discontented with 1% based on the non-conductorization of aging defective part, the failure rate height, more than 1%, failure rate reduces equably.Therefore, for making the defective part oxidation by aging, realize non-conductorization, aging process is preferably in organic EL S1 is placed under the state in the atmosphere of oxygen concentration more than 1% and carries out.
This is external to possess has by enclosing under the occasion of gas with the element sealing process of organic EL S1 sealing, implements aging process before being preferably in the element sealing process.
At this wherein, the oxygen concentration of the inclosure gas that uses in the element sealing process is in below the oxygen concentration in the aging process.Specifically, the oxygen concentration of enclosing gas is in below 1%.It is based on following reason.
In organic EL, the dark space became a problem in the past.So-called dark space means the non-luminous region that is undertaken by pixel edge in time.Become problem in the panel quality based on the brightness decline of dark space and bad order.
The present inventor carries out the element sealing process to carried out aging organic EL S1 in the atmosphere of oxygen concentration 1%, changes the oxygen concentration of the inclosure gas of this moment, has investigated the degree of carrying out of dark space.Fig. 9 represents this result's one example.
Fig. 9 be expression to by 0,1,4% filling the organic EL of oxygen concentration of sealing gas, at the accompanying drawing of the dark space size of normal temperature standing time.So-called dark space size means the distance of leaving pixel edge.As shown in Figure 9, the degree of carrying out of finding out the dark space depends on oxygen concentration.That is,, except the water of report before this, think that oxygen also is one of major reason as the occurrence cause of dark space.
According to result shown in Figure 9, we can say in addition, that is, the oxygen concentration of the inclosure gas of using in the element sealing process is in below the oxygen concentration in the aging process, then can do one's utmost to suppress the carrying out of dark space if oxygen concentration is below 1%.
Like this, under the occasion that possesses the element sealing process, as shown in Figure 8, before the element sealing process, implement aging process, and the oxygen concentration that makes the inclosure gas that uses in the element sealing process is in below the oxygen concentration in the aging process, be in especially below 1%, can realize thus implementing burin-in process well, and suppressed the manufacturing of organic EL of the generation of dark space.
In addition in the present embodiment, make applying between the disintegration voltage that voltage is in the disintegration voltage of defective part and organic EL in the burin-in process, but more than the back voltage (anti-bias voltage) when preferably making applying voltage and be in actual driving of organic EL S1 in the burin-in process.
In organic EL, the back voltage during actual the driving is set to usually based on the para-electric of luminosity specification and presses above value.This is because under the occasion that organic EL is used for the dot matrix driving, for preventing that back voltage one side is necessary to press greater than para-electric based on crosstalking that this dot matrix drives.
Therefore, the viewpoint of the capable defective from more positively prevent actual driving, the above enforcement of back voltage during applying voltage and be preferably in actual driving in the burin-in process.
Specifically, under the occasion of the disintegration voltage of the disintegration voltage＜organic EL of the back voltage＜defective part when the magnitude relationship of each voltage satisfies actual the driving, burin-in process is implemented between the disintegration voltage of the disintegration voltage of defective part and organic EL.
Under the occasion of the disintegration voltage of the back voltage＜organic EL the when disintegration voltage of this external defective part＜reality drives, burin-in process is implemented between the disintegration voltage of actual driving voltage and element.In any occasion, in the burin-in process apply the back voltage of voltage when reality drives more than implement.
On the basis of the back voltage that this is external when having determined actual drive of organic EL S1 according to the principle more than the disintegration voltage that is in defective part, more than the back voltage when preferably making applying voltage and be in actual driving of organic EL S1 in the burin-in process.
Like this, in the organic EL S1 that is finished, the back voltage during actual the driving is in applying below the voltage in the burin-in process, and is in more than the disintegration voltage of defective part.That is, the back voltage when driving by reality can approach the processing of burin-in process.
Therefore, even taken place under the occasion of new defective part, when reality drives, also can make defective part open circuit destruction in the occasion that defective part open circuit is destroyed and in the later operation of burin-in process and in using.
Such as, though the back voltage 20V when driving with 85 ℃ has driven and applied voltage by 21V and carry out a plurality of organic ELs that burin-in process produces, even organic EL was through 2000 hours arbitrarily, the row defective does not take place yet, can realize high reliability.
(execution mode 2)
According to present inventor's discussion, find out that the disintegration voltage of organic EL and the thickness t of the organic membrane in the organic EL have correlation.In the organic EL S1 that produces according to process flow chart shown in Figure 2, thickness t (nm) and the disintegration voltage (V) of organic EL S1, the relation of destruction electric field strength (MV/cm) of organic membrane 4～6 have been done investigation.
Figure 10 represents its result.Here, the thickness t of organic membrane comprises under the occasion of conductive films 3 such as CuPc in organic membrane 3～6, is the thickness t that has removed the organic membrane 4～6 of this conductive film.Why removing this conductive film, is that its resistance value is minimum because this conductive film is compared with other organic membrane, and how electric field is not applied.
That is, in Figure 10, change the thickness t of the organic membrane 4～6 of removing the hole injection layer of forming by CuPc 3, according to measuring the disintegration voltage that the same main points of operation have been obtained organic EL S1 with above-mentioned disintegration voltage.The destruction electric field strength of organic EL S1 is the disintegration voltage of the organic EL S1 that will the be obtained result after divided by the thickness t of organic membrane 4～6 in addition.Measure in addition and carry out at normal temperatures.
According to result shown in Figure 10, the disintegration voltage of discovery organic EL S1 depends on the thickness t of organic membrane 4～6, and is relative therewith, destroys the thickness t that electric field strength does not depend on organic membrane 4～6, almost certain.
Like this, to a plurality of organic EL S1, investigated the destruction electric field strength of organic EL S1 (normal portion) equally.Figure 11 represents this result as the distribution of this destruction electric field strength.
As shown in figure 11, finding that its mean value of destruction electric field strength of organic EL S1 is 3.9MV/cm, is 3.2MV/cm as the lower limit of 3 σ.
Therefore in the present embodiment, when the back voltage with the actual driving of organic EL S1 the time is made as R, if the value between this back voltage R and (t * 3.9) MV/cm is made as the voltage range that applies in the burin-in process, then normal portion is that organic EL S1 does not destroy, and the defective part open circuit is destroyed.
Here, if the value between above-mentioned back voltage R and (t * 3.2) MV/cm is made as the voltage range that applies in the burin-in process, the destruction that then can prevent organic EL is more reliably wished so.
Therefore according to present embodiment, also can provide a kind of and the normal portion of element not caused damage, and make the defective part method for manufacturing organic EL destroyed of open circuit suitably in advance.
(execution mode 3)
Embodiment of the present invention 3 relates to manufacture method, and is in the aging process in carrying out process flow chart shown in Figure 2, additional for making defective part carry out the operation of heat treated to organic EL S1 than more obviousization of room temperature state.
Make defective part obviously change the discussion result of this point by heat treated based on present inventor of following record etc.
At first, proceed to anode and form operation, surface treatment procedure, organic membrane formation operation, negative electrode formation operation, element sealing process, formed and above-mentioned same organic EL S1.This element S1 is identical with the structure of the display floater of a structure example shown in Figure 1.
That is, this element S1 also on glass substrate 1 successively lamination as the ITO film 2 of the thickness 140nm of anode, as the CuPc film 3 of the thickness 50nm of hole injection layer, as the TPTE film 4 of the thickness 60nm of hole transporting layer, as the doping of the thickness 40nm of luminescent layer the Alq of 1% dimethyl quinoline a word used for translation ketone
3Film (Alq
3Luminescent film) 5, as the Alq of the thickness 20nm of electron supplying layer
3Film 6, as the LiF film 7 of the thickness 0.5nm of electron injecting layer, as the Al film 8 of the thickness 100nm of negative electrode.Like this, this element S1 constitutes 256 * 64 rectangular pixels.
Carried out this organic EL S1 is placed the so-called high temperature placement of 2hr in 120 ℃ temperature.Like this, in this element S1, before high temperature is placed,, investigated and applied voltage-to-current density feature (V-I characteristic) with afterwards.Figure 12 represents its result.In Figure 12, the transverse axis representative applies voltage, vertical axis represents current density, the V-I characteristic X II B after the V-I characteristic X II A before expression high temperature is placed, acceleration high temperature are placed.
In Figure 12, before high temperature was placed, expression was to apply voltage 4V as threshold value, the so-called normal V-I characteristic that current density rises when applying the voltage rising.But after high temperature is placed, leakage current and short circuit take place, having found has unusual that bigger electric current flows being lower than applying of threshold value under the voltage.
This phenomenon is further explored, with microscopic examination the organic membrane surface among the organic EL S1 promptly as the above-mentioned Alq of electron supplying layer
3The surface of film 6.Figure 13 represents this observed result as the pattern sectional drawing based on microphotograph.
In Figure 13, on ITO film 2, lamination has CuPc film 3, TPTE film 4, Alq successively
3 Luminescent film 5, Alq
3Film 6, (a) after 85 ℃ of placements of expression, (b) after 100 ℃ of placements of expression, (c) state after 120 ℃ of placements of expression.As shown in figure 13, laying temperature rises more, more at Alq
3The surface observation of film 6 infers that to more space B the formation that this space B is relevant with leakage current.
The size of this space B is represented as the depth of interstices D shown in Figure 13, represented the curve of the temperature dependency of this depth of interstices D among Figure 14.Found temperature dependency in the size of space B, the formation threshold temperature of judging space B from the extrapolated value of curve is 70 ℃.
When being heated to 85 ℃, sinking in (space) of degree of depth 35nm appears, and under the occasion that has applied voltage, at this position of sinking voltage takes place and concentrate, infer the reason that this is above-mentioned leakage current shown in Figure 12.
According to foregoing, be in the condition of high temperature by making organic EL, defective part such as the space that exists in the film are grown up more than room temperature state, become remarkable.That is,, the defective part of the possibility with timeliness generation is obviously changed, can be found reliably by being in the condition of high temperature.
Here, in organic EL, the organic membrane structure material is mostly by the vacuum vapour deposition film forming, can roughly be divided into when its film forming the vapo(u)rability material that gasifies via liquid from solid and from the sublimability material of solid direct gasification.Therefore, according to present inventor's etc. discussion, by heat treated make obviousization of defective part in this point at above-mentioned Alq
3Significantly occur in the sublimability material.Think that this is that it is interparticle less in conjunction with energy because sublimability material one side compares with the vapo(u)rability material, thereby more easily produce the space.Therefore, as shown in figure 14, infer to be tending towards high temperature more that it is big more that the space becomes, the electrical leak between electrodes stream in the element also increases simultaneously.
According to above-mentioned discussion, in present embodiment 3, be provided to making defective part carry out carrying out the manufacture method of aging process after the heat treated to organic EL S1 than more obviousization of room temperature state.Figure 15 represents concrete process flow chart.
The manufacture method of present embodiment 3 shown in Figure 15 is a kind of in above-mentioned manufacture method shown in Figure 2, carries out the method for heating treatment step between element sealing process and aging process.It is to carry out in 70 ℃～120 ℃ the scope that this heating treatment step is preferably in its treatment temperature.
This be because, as above-mentioned shown in Figure 14, the threshold temperature the when space forms is 70 ℃, if since the growth of 70 ℃ of defective part such as space with on the other hand after above 120 ℃, then the cause thermal damage of element itself will increase.
According to manufacture method shown in Figure 15, organic EL S1 is carried out heat treated, can make the defective part than more obviousization of room temperature state, by the aging process that after this carries out, this defective part of obviously having changed open circuit is destroyed.
Under the occasion of this external not heat treated, before aging process, it is not clear clear to constitute the defective part that exists in the film 2～8 of organic EL S1.In contrast to this, under the occasion of having carried out heat treated, even the defective part that heat treated not just can not occur takes place, this defective part destruction of also can opening a way.
That is, present embodiment 3 is a kind of defective part when making, also for the defective part with possibility that timeliness takes place, the manufacture method that also can open a way reliably in advance and destroy.Therefore, can further realize the organic EL that reliability is high.
With reference to Figure 16 the concrete effect of present embodiment 3 is explained.Figure 16 is the chart of the result of the test of turning on light continuously of the organic EL S1 that produced by above-mentioned manufacture method shown in Figure 15 of expression.
Turning on light continuously test among Figure 16 be one in above-mentioned manufacture method shown in Figure 15, proceeding to the panel of aging process, implemented the tests of the test of turning on light continuously in 85 ℃ of thermostats.This panel is the display floater with 256 * 64 matrix pixel structures.
Like this, heating treatment step heats in 85 ℃ baking oven by the element (panel) that will proceed to sealing process and carried out in 60 minutes.Then, element is taken out in baking oven, as applying waveform, utilize 125Hz, the rectangular pulse of 1/64 duty (applies 1 time along bias voltage 12V, then applies 63 anti-bias voltages-25V), carried out 1 minute burin-in process.
The row defective (in the test of turning on light continuously (85 ℃ of atmosphere) of the panel number A6 among Figure 16～A10) carry out, as shown in figure 16, even through 500 hours, is also all being taken place in the display floater that provides in this heat treated and aging process.
That is, in present embodiment 3, can confirm to compare, can realize that row defective time of origin further prolongs, and has the more organic EL of high reliability with organic EL shown in Figure 5.
As the variation of present embodiment 3, can after heat treated, not wear out in addition yet, and carry out heat treated simultaneously with aging.That is, also can be for making defective part carry out organic EL S1 carrying out aging process under the state of heat treated than more obviousization of room temperature state.
Figure 17 represents the process flow of the manufacture method of this variation.In this variation, specifically, the organic EL S1 that has proceeded to the element sealing process was heated 60 minutes in 85 ℃ baking oven, in 85 ℃ baking oven, keep, utilize above-mentioned 125Hz, the rectangular pulse of 1/64 duty carries out 1 minute burin-in process.
Under this occasion, also 5 display floaters have been carried out the test of turning on light continuously under above-mentioned 85 ℃, as the result identical with above-mentioned Figure 11, though in any one panel through the row defective also took place in 500 hours.That is,, reach under the aging occasion, also can realize the action effect of present embodiment 3 even carry out heat treated at the same time according to this variation.
In addition as mentioned above, make defective part obviously change this point by heat treated at above-mentioned Aiq
3And so on the sublimability material in obviously occur.For this reason, preferably adopt at least a or whole film forming that make the constituent material of the organic membrane 3～6 in the organic EL by vacuum vapour deposition, when its film forming, the raw material that have by organic membrane gasify via liquid from solid, the material of the so-called vapo(u)rability of film forming on substrate.
Like this,, the generation in above-mentioned space can be reduced, consequently, the generation of defective part can be reduced by in the constituent material of organic membrane at least a, adopting the vapo(u)rability material.
Among the organic EL S1 shown in this external above-mentioned configuration example, the luminescent layer 5 in the organic membrane 3～6, electron supplying layer 6 are by the Alq as oxine aluminium complex
3Form.This Alq
3Be a kind of by the vacuum vapour deposition film forming, when its film forming, have raw material by the organic membrane sublimability material of the so-called sublimability of film forming from the solid direct gasification and on substrate.
Like this, when the constituent material of organic membrane at least a was the sublimability material, the treatment temperature in the heat treated preferably was in this sublimability material and is taken place more than the temperature of metamorphosis by heat.
Like this, be when being easy to produce the sublimability material in space the constituent material of organic membrane at least a, by heat treated, the metamorphosis that can be easy to take place the sublimability material is space etc., and defective part is obviously changed.
In addition as mentioned above, to be preferably in its treatment temperature be to carry out in 70 ℃～120 ℃ the scope to the heating treatment step of present embodiment.This is corresponding at the Alq as the sublimability material
3In the film 6 (electron injecting layer 6), reach more than 70 ℃ after, the growth of defective part such as space just begins.
(execution mode 4)
But, the qualification rate of burin-in process depends on the defective incidence that aging process is later.Especially be necessary to prevent reliably the generation of defective in market.
For this reason, establishing the good of burin-in process denys that criterion just necessitates.Present embodiment provides a kind of very manufacture method of criterion not of burin-in process that possessed.Figure 18 represents the process flow of the manufacture method of present embodiment.The good operation of not judging of carrying out burin-in process is that leakage current is judged operation.
This criterion is judged the good of burin-in process based on the leakage current that flows between anode 2 and negative electrode 8 when organic EL S1 has been applied back voltage after burin-in process.Such as, in judgement, the upper limit of very denying determinating reference can be made as 5 * 10 based on leakage current
-2A/m
2
Below the expression leakage current is judged the specific embodiment of operation.At first, to 32760 organic ELs (pixel) S1, the defective part open circuit is destroyed by the burin-in process in the aging process.Judge in the operation at leakage current then, between anode 2 and negative electrode 8, applied the back voltage (anti-bias voltage) of 15V.
Like this, in the most normal portion that comprises the ruinate defective part of opening a way, leakage current density is in 1 * 10
-2A/m
2Below.Relative therewith, aging bad in part, it is in bad that non-luminous non-luminous generating device (pixel) has taken place, and all leakage current densities are in 5 * 10
-2A/m
2More than.
Figure 19 is that (the element number F1 among Figure 19～F7) has represented the chart of leakage current density to 7 in this bad (non-luminous generating device).To 7 all bad portions, leakage current density is 5 * 10
-2A/m
2More than.Like this, when these bad portions had carried out 1000 hours action test under 85 ℃, it was non-luminous that short circuit has all taken place.
Therefore, after burin-in process,, judge the good of burin-in process, can carry out the good of burin-in process thus and not judge based on the leakage current that when organic EL S1 has been applied back voltage, between anode 2 and negative electrode 8, has flowed.That is,, can carry out changing into the non-defective unit and the unsuccessful difference that the defective products of short circuit has taken place of merit clearly by aging open a way destruction and non-conductor according to the above-mentioned leakage current of measuring after the burin-in process.
(other execution mode)
In addition, under the occasion that anode 2 is made up of indium tin oxide (ITO), preferably its average surface roughness Ra is below the 2nm, and 10 average surface roughness Rz are below the 20nm.These Ra, Rz stipulate in JIS (Japanese Industrial Standards).
Disintegration voltage also depends on the surface roughness of anode 2.Because anode is made up of ITO (indium tin oxide) usually, thereby by the surface roughness of this ito anode is done above-mentioned setting, almost can ignore the destruction that is caused by this surface roughness, can carry out burin-in process reliably.
In addition as organic EL, as substrate, anode, organic membrane, negative electrode etc., except above-mentioned material, can also suit to adopt be used for organic EL or have a material that uses possibility.
Claims (16)
1. method for manufacturing organic EL, it possesses the operation that is formed on the organic EL (S1) that wrapped folder organic membrane (3～6) forms between anode (2) and the negative electrode (8);
In above-mentioned organic EL, carry out between above-mentioned anode and above-mentioned negative electrode, applying the burin-in process of voltage, make the aging process of the defective part open circuit destruction that exists in the film,
It is characterized in that:
After the electric current that flows when having applied anti-bias voltage by being determined in the above-mentioned organic EL, the open circuit of having obtained above-mentioned defective part destroy the voltage range that takes place and above-mentioned organic EL and produce the voltage range of destroying,
The open circuit of this defective part destroyed minimum voltage and organic EL in the voltage range that takes place produces the voltage range between the minimum voltage in the voltage range of destroying and the voltage range more than the back voltage absolute value when being the actual driving of above-mentioned organic EL, as the scope that applies voltage in the above-mentioned burin-in process, carry out above-mentioned aging process.
In the claim 1 record method for manufacturing organic EL, it is characterized in that:
The open circuit of above-mentioned defective part destroyed between the minimum voltage in the voltage range that maximum voltage and above-mentioned organic EL (S1) in the voltage range that takes place produce destruction as the scope that applies voltage in the above-mentioned burin-in process.
In the claim 1 record method for manufacturing organic EL, it is characterized in that:
Above-mentioned defective part open circuit is destroyed between the maximum voltage in the voltage range that minimum voltage and above-mentioned defective part open circuit in the voltage range that takes place destroy generation as the scope that applies voltage in the above-mentioned burin-in process.
Claim 1 to 3 arbitrary in the record method for manufacturing organic EL, it is characterized in that:
On the basis of the back voltage the when principle more than the peaked absolute value of the voltage range that destroy to take place according to the open circuit that reaches above-mentioned defective part has determined that above-mentioned organic EL (S1) is actual and drives, more than the back voltage absolute value when making applying voltage and be in the actual driving of above-mentioned organic EL in the above-mentioned burin-in process.
In the claim 1 record method for manufacturing organic EL, it is characterized in that:
For making above-mentioned defective part carry out carrying out above-mentioned aging process after the heat treated to above-mentioned organic EL (S1) than more obviousization of room temperature state.
In the claim 1 record method for manufacturing organic EL, it is characterized in that:
For when making above-mentioned defective part carry out heat treated to above-mentioned organic EL (S1), carry out above-mentioned aging process than more obviousization of room temperature state.
In the claim 5 record method for manufacturing organic EL, it is characterized in that:
At least a of the constituent material of above-mentioned organic membrane (3～6) is by the vacuum vapour deposition film forming, has the material of vapo(u)rability.
In the claim 5 record method for manufacturing organic EL, it is characterized in that:
At least a of constituent material at above-mentioned organic membrane (3～6) is by the vacuum vapour deposition film forming, when having the sublimability material of sublimability,
Treatment temperature in the above-mentioned heat treated is in above-mentioned sublimability material and is taken place more than the temperature of metamorphosis by heat.
In the claim 8 record method for manufacturing organic EL, it is characterized in that:
Above-mentioned sublimability material is an oxine aluminium complex.
In the claim 5 record method for manufacturing organic EL, it is characterized in that:
Treatment temperature in the above-mentioned heat treated is 70 ℃～120 ℃.
11. the method for manufacturing organic EL of record in the claim 1 is characterized in that:
In above-mentioned aging process, implement respectively along bias voltage apply, anti-bias voltage applies.
12. the method for manufacturing organic EL of record in the claim 1 is characterized in that:
Above-mentioned aging process carries out under the state that above-mentioned organic EL (S1) is placed in the atmosphere of oxygen concentration more than 1%.
13. the method for manufacturing organic EL of record in the claim 1 is characterized in that:
Possess by the element sealing process of inclosure gas above-mentioned organic EL (S1) sealing,
Before the said elements sealing process, implement above-mentioned aging process, and the oxygen concentration of the above-mentioned inclosure gas that uses in the said elements sealing process is in below the oxygen concentration in the above-mentioned aging process.
14. the method for manufacturing organic EL of record in claim 1 or 3 is characterized in that:
After above-mentioned burin-in process,, judge the good of above-mentioned burin-in process based on the leakage current that when above-mentioned organic EL (S1) has been applied back voltage, between above-mentioned anode (2) and above-mentioned negative electrode (8), has flowed.
15. the method for manufacturing organic EL of record in the claim 14 is characterized in that:
In judgement, the upper limit of non-defective unit determinating reference is made as 5 * 10 based on above-mentioned leakage current
-2A/m
2
16. the method for manufacturing organic EL of record in the claim 1 is characterized in that:
Above-mentioned anode (2) is made up of indium tin oxide, and its average surface roughness Ra is below the 2nm, and 10 average surface roughness Rz are below the 20nm.
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| JP370579/2002 | 2002-12-20 | ||
| JP370579/02 | 2002-12-20 | ||
| JP2002370579A JP3562522B2 (en) | 2002-01-15 | 2002-12-20 | Manufacturing method of organic EL device |
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| CN100440578C true CN100440578C (en) | 2008-12-03 |
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| CN103646878B (en) * | 2013-12-25 | 2017-01-25 | 鲁东大学 | Method for eliminating defects in lighting layer of film electric lighting device through electric field |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09120890A (en) * | 1995-10-27 | 1997-05-06 | Mitsubishi Chem Corp | Organic electric field fluorescent element and its manufacture |
| JP2001313170A (en) * | 2000-05-01 | 2001-11-09 | Toyota Motor Corp | Organic el element and manufacturing method of the same |
| CN1350417A (en) * | 2000-10-10 | 2002-05-22 | 株式会社半导体能源研究所 | Method for manufacturing and/or repairing lighting equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09120890A (en) * | 1995-10-27 | 1997-05-06 | Mitsubishi Chem Corp | Organic electric field fluorescent element and its manufacture |
| JP2001313170A (en) * | 2000-05-01 | 2001-11-09 | Toyota Motor Corp | Organic el element and manufacturing method of the same |
| CN1350417A (en) * | 2000-10-10 | 2002-05-22 | 株式会社半导体能源研究所 | Method for manufacturing and/or repairing lighting equipment |
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