WO2005122702A2 - 有機エレクトロルミネセンス素子、その検査装置及び検査方法 - Google Patents
有機エレクトロルミネセンス素子、その検査装置及び検査方法 Download PDFInfo
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/12—Light sources with substantially two-dimensional radiating surfaces
- H05B33/14—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of the electroluminescent material, or by the simultaneous addition of the electroluminescent material in or onto the light source
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- G—PHYSICS
- 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
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- G—PHYSICS
- 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
- G09G3/20—Control arrangements or circuits, of interest only in connection with visual indicators other than cathode-ray tubes for presentation of an assembly of a number of characters, e.g. a page, by composing the assembly by combination of individual elements arranged in a matrix no fixed position being assigned to or needed to be assigned to the individual characters or partial characters
- G09G3/22—Control arrangements or circuits, of interest only in connection with visual indicators other than cathode-ray tubes for presentation of an assembly of a number of characters, e.g. a page, by composing the assembly by combination of individual elements arranged in a matrix no fixed position being assigned to or needed to be assigned to the individual characters or partial characters using controlled light sources
- G09G3/30—Control arrangements or circuits, of interest only in connection with visual indicators other than cathode-ray tubes for presentation of an assembly of a number of characters, e.g. a page, by composing the assembly by combination of individual elements arranged in a matrix no fixed position being assigned to or needed to be assigned to the individual characters or partial characters using controlled light sources using electroluminescent panels
- G09G3/32—Control arrangements or circuits, of interest only in connection with visual indicators other than cathode-ray tubes for presentation of an assembly of a number of characters, e.g. a page, by composing the assembly by combination of individual elements arranged in a matrix no fixed position being assigned to or needed to be assigned to the individual characters or partial characters using controlled light sources using electroluminescent panels semiconductive, e.g. using light-emitting diodes [LED]
- G09G3/3208—Control arrangements or circuits, of interest only in connection with visual indicators other than cathode-ray tubes for presentation of an assembly of a number of characters, e.g. a page, by composing the assembly by combination of individual elements arranged in a matrix no fixed position being assigned to or needed to be assigned to the individual characters or partial characters using controlled light sources using electroluminescent panels semiconductive, e.g. using light-emitting diodes [LED] organic, e.g. using organic light-emitting diodes [OLED]
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/70—Testing, e.g. accelerated lifetime tests
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
- H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
- H10K85/115—Polyfluorene; Derivatives thereof
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
- H10K85/151—Copolymers
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- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09G—ARRANGEMENTS OR CIRCUITS FOR CONTROL OF INDICATING DEVICES USING STATIC MEANS TO PRESENT VARIABLE INFORMATION
- G09G2320/00—Control of display operating conditions
- G09G2320/04—Maintaining the quality of display appearance
- G09G2320/043—Preventing or counteracting the effects of ageing
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
Definitions
- the present invention relates to an organic electroluminescence element, an inspection device and an inspection method thereof, and an organic electroluminescence display device. More specifically, an organic electroluminescence element used as an electroluminescent element in an organic electroluminescent display, an inspection apparatus and an inspection method suitable for inspecting the life characteristics thereof, and an organic electroluminescence display apparatus It is about. Background art
- Light-emitting materials used for organic EL devices include low-molecular-weight organic EL materials and high-molecular-weight organic EL materials.
- a typical organic EL device using a polymer organic EL material is, for example, a transparent anode made of indium tin oxide (hereinafter, also referred to as “ITO”) on a glass substrate, a PEDOT / PSS A hole transport layer composed of ⁇ Poly (ethylene-dioxythiophene) / Poly (styrenesulfonate); a light-emitting layer composed of a polymer organic EL material; and CaZAl.
- the cathode has a structure that is sequentially laminated.
- an organic EL device having such a structure can achieve a luminance of 100000 cdZm 2 or more, a luminous efficiency of several lmZW to several tens of lmZW, and a lifetime of several thousand to tens of thousands of hours.
- Such a conventional organic EL element has sufficiently high luminance and luminous efficiency, but its life is not sufficient in view of application to an actual product, and its application range is limited. there were. Therefore, various measures have conventionally been investigated to improve the life characteristics of the organic EL element. For example, techniques for improving the luminescent material itself (for example, see Patent Document 1) and improving the cathode (for example, see Non-Patent Document 1) have been proposed. However, even if these measures are taken, organic EL displays must be modified in order to obtain a practical and versatile organic EL device with an extremely short lifespan compared to other FPDs that use liquid crystals. There was room for good.
- Patent Document 1 Japanese Patent Publication No. 11-508731 (pages 1 and 2) (corresponding to International Publication No. 97/40648 pamphlet and US Pat. No. 6,326,091)
- Non-Patent Document l Yong Cao, et al., "Ultrathin layer alkaline earth metals as stable electron— injecting electrodes for polymer light emitting dio des) J, JOURNAL OF APPLIED PHYSICS, USA, September 15, 2000, Vol. 88, No. 6, p. 3618
- Non-Patent Document 2 Kenichi Koshi, et al., "The Unique Emission Characteristics of Ir (ppy) 3 at Low Temperatures," Applied Physics Society Academic Lecture 2003 Spring, p. 1412, 28p -A-4
- Non-Patent Document 3 Kenichi Koshi and three others, "Examination of exciton diffusion length of Ir (ppy) 3", Japan Society of Applied Physics, Academic Lecture 2003 Autumn, p. 1206, la-YL- 7
- the present invention has been made in view of the above situation, and an organic electroluminescent device having excellent life characteristics, and a device for easily inspecting the life characteristics in a short time without deteriorating the device. It is an object of the present invention to provide a device and a method for testing an organic electroluminescence element, and a method for testing an organic electroluminescence display device.
- the PL intensity at 300K should be higher than the PL intensity at any temperature lower than 300K to achieve a long-life organic EL device.
- the present inventors have found that it is possible to perform element defect sorting without deteriorating the element only by measuring the initial characteristics, and conceived that the above problem can be solved brilliantly, and reached the present invention. is there.
- the present invention relates to an organic electroluminescence device having a structure in which at least one or more organic layers including at least a light emitting layer are sandwiched between electrodes, wherein the organic electroluminescent device has a photoluminescence at 300K.
- the organic electroluminescence (EL) element of the present invention has a structure in which at least one or more organic layers including at least a light emitting layer are sandwiched between electrodes.
- the light emitting layer that constitutes such an organic EL element is a layer that contains an organic material that emits light when an electric field is applied.
- the organic layer has a structure in which layers including an organic material such as a light emitting layer are laminated, and usually includes a hole injection layer, a hole transport layer, an electron transport layer, and the like in addition to the light emitting layer. It is a thing.
- Preferred embodiments of the organic EL device of the present invention include, for example, an embodiment in which a substrate, an anode, a hole transport layer, a light emitting layer, and a cathode are stacked in this order. At this time, it is preferable that at least one of the anode and the cathode has translucency.
- the organic EL device of the present invention is not particularly limited as long as such components are formed as essential components, and may or may not include other components.
- the organic EL device of the present invention having the above-described configuration can emit light by applying an electric field between the electrodes, and usually emits light by applying an AC electric field or the like.
- the organic electroluminescent element has a photoluminescence intensity at 300K of less than 30 OK! /, Which is stronger than the photoluminescence intensity at a certain temperature.
- An organic EL device exhibiting such temperature dependence in photoluminescence intensity (PL intensity) can be suitably used as an electroluminescent device of an organic EL display because of its excellent life characteristics.
- a more preferred form includes a form in which the PL strength at 300K is stronger than the PL strength at any temperature of less than 200K, and a more preferred form is a PL form at any temperature where the PL strength at 300K is less than 300K. Forms that are stronger than strength are mentioned.
- photoluminescence means a fluorescent phenomenon caused by stimulation with light such as ultraviolet light, visible light, and infrared light.
- the PL intensity means energy or the number of photons emitted as fluorescence in a wavelength range of 380 to 780 nm (visible region) per unit time, and can be measured by using a strike scope, a spectroscope, or the like.
- the organic electroluminescent element has a photoluminescence intensity at 300K higher than a photoluminescence intensity at 5K.
- the organic EL element having such characteristics surely has excellent life characteristics. This is because the temperature dependence of the PL intensity of a light-emitting material depends largely on the temperature dependence of the heat deactivation process of the material.Some of the materials have such a heat deactivation process that becomes noticeable for the first time at a temperature near absolute zero. Therefore, by measuring the temperature dependence of the PL intensity of the organic EL device and comparing the PL intensity measured at 300K with the PL intensity measured at cryogenic conditions of about 5K, the life characteristics of the device can be more accurately determined. Because it can be sought.
- the above-mentioned organic electroluminescence element defines the photoluminescence intensity at 5K when the photoluminescence intensity at 300K is 1, as the low-temperature photoluminescence intensity ratio.
- the photoluminescence intensity ratio Y represented by the following formula (1) is 1 or less.
- ⁇ (low-temperature photoluminescence intensity ratio of organic electroluminescent element) / (low-temperature photoluminescence intensity ratio of light-emitting layer) (1)
- the PL intensity ratio ⁇ represented by the above formula (1) being 1 or less means that the low-temperature photoluminescence intensity ratio of the organic EL element is smaller than the low-temperature photoluminescence intensity ratio of the light emitting layer. I do. Therefore, the organic EL device having such characteristics has a device configuration suitable for improving the life characteristics, and is particularly excellent in the life characteristics.
- the PL intensity ratio Y is more preferably 0.5 or less.
- the low-temperature PL intensity ratio of the light-emitting layer shown in the above formula (1) is the same as that of the light-emitting layer of the organic EL element. Can be obtained by measuring the low-temperature PL intensity ratio.
- the photoluminescence of the organic electroluminescent element includes two or more fluorescent components having substantially the same emission stadium and having different lifetimes, and the two or more fluorescent components include: In any case, it is preferable that the photoluminescence intensity at 300K is stronger than the photoluminescence intensity at any temperature lower than 300K. As a result, an organic EL device having particularly excellent life characteristics can be provided.
- a more preferred form is a form in which the PL intensity at 300K is less than 200K for all of the two or more fluorescent components, and the PL intensity at a certain temperature is stronger than the PL intensity at a certain temperature.
- the PL intensity at 300K is stronger than the PL intensity at all temperatures lower than 300K.
- including two or more fluorescent components means that there are two or more light emission mechanisms, that is, two or more relaxation processes due to fluorescence from a photo-excited state. Further, that the two or more fluorescent components have substantially the same emission spectrum means that the shapes of the emission spectra derived from the respective emission mechanisms are substantially the same. Further, that the lifespan of two or more fluorescent components is different means that the fluorescence intensity half-lives of the fluorescent components derived from each light emission mechanism are different. Therefore, the organic EL device containing the two or more fluorescent components When graphing the fluorescence intensity of logarithmic notation on the ordinate and the elapsed time of linear notation on the abscissa, the attenuation characteristic of PL intensity is curved.
- the PL intensity at 300K of each of the two or more fluorescent components is stronger than the PL intensity at 5K.
- An organic EL device having such characteristics has particularly excellent life characteristics more reliably.
- the present invention also relates to an apparatus for inspecting the life characteristics of an organic electroluminescent element, wherein the apparatus for inspecting an organic electroluminescent element comprises a light emitting material constituting a light emitting layer of the organic electroluminescent element.
- a light source to be excited detection means for detecting the photoluminescence intensity of the organic electroluminescence element, temperature control means for controlling the temperature of the organic electroluminescence element and Z or the vicinity thereof, and a photometer measured by the detection means.
- the present invention also provides an inspection device for an organic electroluminescent device, which includes a data storage unit for storing luminescence intensity and a data processing unit for comparing photoluminescence intensity measured at different temperatures.
- the light source is not particularly limited.
- a laser device that emits laser light having a central wavelength of 325, 337, or 365 nm, or only a light having an excitation wavelength that is optimal for a light-emitting material by a white light power monochromator is used.
- a light source device that takes out and emits light is used.
- the detection means is not particularly limited as long as it can detect the PL intensity of the organic EL element photo-excited by the light emitted from the light source, and may be a device that monitors a photocurrent with a photodiode or a spectroscope. An apparatus that monitors the PL intensity using the area of the measured fluorescence spectrum may be used.
- the temperature control means is not particularly limited, and examples thereof include a device that includes a cooling unit and a heater and controls the output of the cooling unit and the heater to an arbitrary temperature, a control device that uses a cryostat, and the like.
- the data storage means is not particularly limited as long as it can store the data obtained by the detection means.
- the data processing means is particularly limited as long as it can compare the PL intensities of the organic EL elements measured at different temperatures using the data stored in the data storage means. Not something.
- the life characteristics of the organic EL element can be inspected without performing an aging test, and the life can be easily and simply reduced without deteriorating the element. It is possible to select elements having poor characteristics.
- by developing an organic EL device using such an inspection device it is possible to optimize the configuration conditions of the device, manufacturing process conditions, etc. with respect to the selection of the light emitting material and the design of the film thickness of the film constituting the device. Can be easily performed.
- a preferred form of the organic EL element inspection apparatus of the present invention a form in which the PL intensity of the organic EL element measured at 300K and the PL intensity of the organic EL element measured at 5K are compared by data processing means is used.
- the life characteristics of the element can be measured with higher accuracy.
- the inspection apparatus for an organic EL element of the present invention may be a form in which a light source and each means are combined with each other.
- a data storage means and a data processing means are combined and integrated. It may be in a form or the like.
- the present invention further relates to a method for inspecting the life characteristics of an organic electroluminescent element, wherein the method for inspecting an organic electroluminescent element includes a method for inspecting the photoluminescence of the organic electroluminescent element at at least two different temperatures. It is also a method of inspecting an organic electroluminescent device, which detects the intensity and also inspects the life characteristics of the organic electroluminescent device.
- the life characteristics of the organic EL device can be tested without performing an aging test, and a device having a poor life characteristic can be easily obtained in a short time without deteriorating the device. Sorting can be performed.
- by developing an organic EL device using such an inspection device it is possible to optimize the element configuration conditions, manufacturing process conditions, etc. with respect to the selection of the light emitting material and the design of the film thickness of the device. Can be easily performed.
- the present invention is also an organic electroluminescence element obtained by using the above-described organic electroluminescence element inspection apparatus or the above-described organic electroluminescence element inspection method.
- Such an organic EL element is obtained after performing a high-precision sorting on the life characteristics by using the organic EL element inspection apparatus or the organic EL element inspection method. It has excellent life characteristics and can be suitably used as an electroluminescent element of an organic EL display.
- the present invention is also an organic electroluminescent display device provided with the organic electroluminescent element.
- Such an organic EL display organic EL display
- the organic electroluminescence device of the present invention since the photoluminescence intensity at 300 K is higher than the photoluminescence intensity at any temperature lower than 300 K, it is possible to provide a device having a long device life. Can be. Such an organic electroluminescent element having a long element life can be suitably used as an electroluminescent element of an organic electroluminescent display.
- FIG. 1 is a cross-sectional view schematically showing a configuration of the organic electroluminescence (EL) element of the first embodiment.
- EL organic electroluminescence
- the organic EL device of the present embodiment has a structure in which an anode 2, a hole transporting layer 3, a light emitting layer 4, and a cathode 5 are formed on a substrate 1 in that order. ing.
- the organic EL device shown in FIG. 1 is manufactured, for example, by the following method.
- an anode 2 is formed on a substrate 1 having an insulating surface.
- a substrate with an electrode in which an anode 2 made of ITO (indium oxide monooxide) was previously formed on the surface of a glass substrate 1 of 30 mm ⁇ 30 mm square was prepared and washed.
- a method of cleaning the substrate with electrodes for example, a method of performing ultrasonic cleaning for 10 minutes using acetone, isopropyl alcohol (IPA) or the like, followed by ultraviolet (UV) -ozone cleaning for 30 minutes, or the like is used. No. Thereby, the anode 2 is formed.
- a hole transport layer 3 (thickness :, for example, 60 nm) is formed on the surface of the anode 2 by, for example, the following method.
- a coating liquid for forming a hole transport layer is prepared by dispersing PEDOTZPSS in pure water.
- this coating liquid for forming a hole transport layer is applied to the surface of the anode 2 using a spin coater. Thereafter, the solvent in the coating liquid for forming a hole transport layer is removed by heating and drying the substrate with electrodes (200 ° C., 5 minutes) in a high-purity nitrogen atmosphere. Thereby, the hole transport layer 3 is formed.
- a light-emitting layer 4 (thickness: 80 nm, for example) is formed, for example, by the following method.
- a coating solution for forming a light emitting layer is prepared by dissolving a high molecular light emitting material in xylene.
- this light emitting layer forming coating liquid is applied to the surface of the hole transport layer 3 using a spin coater. Thereafter, the solvent in the light emitting layer forming coating liquid is removed by heating and drying in a high purity nitrogen atmosphere. Thereby, the light emitting layer 4 is formed.
- the cathode 5 is formed, for example, by the following method.
- the substrate 1 on which the light emitting layer 4 is formed is fixed to the first metal deposition chamber.
- calcium is deposited on the surface of the light emitting layer 4 by a vacuum evaporation method (thickness: for example, 30 nm), and subsequently, silver is deposited (thickness: for example, 300 nm) by the same method.
- the opposite cathode 5 is formed.
- a sealing glass (not shown) is bonded to the substrate 1 using a UV-curable resin to complete the organic EL element.
- the effect of the present invention was confirmed by fabricating an organic EL device by changing the light emitting material and the process conditions.
- the organic EL device of Example 1 (hereinafter, also referred to as device (1)) was obtained by forming a light-emitting layer 4 by heating and drying a polyfluorene-based green light-emitting material A at a firing temperature of 150 ° C.
- the polyfluorene-based green light-emitting material A is a copolymer of a fluorene ring having an alkyl chain R and R 'and at least one unit of an aromatic aryl ligated unit Ar (Ar').
- the chemical formula is represented by the following formula (A).
- the molecular weight of the polyfluorene-based green light-emitting material A is hundreds of thousands, and the glass transition point differs depending on the unit to be copolymerized.
- R and R ′ represent an alkyl chain
- Ar and Ar ′ represent units of an aromatic aryl compound
- 1, m is an integer of 1 or more
- n is , 0 or an integer of 1 or more.
- Aromatic aryl compounds include dimethylbenzene, pyridine, benzene, anthracene, spirobifluorene, fulvazole units, benzoamine, bipyridine, and benzothiadiazo. Or the like is used.
- the organic EL device of Example 2 (hereinafter, also referred to as device (2)) was obtained by forming a light-emitting layer 4 by heating and drying a polyfluorene-based green light-emitting material A at a firing temperature of 90 ° C.
- the measurement result of the luminance half-life by the aging test of the element (2) was 720 hours at an initial luminance of lOOOOcdZm 2 .
- the organic EL device of Comparative Example 1 (hereinafter, also referred to as device (3)) was obtained by forming a light-emitting layer 4 by heating and drying a polyfluorene-based green light-emitting material B at a firing temperature of 150 ° C.
- the measurement result of the luminance half-life by the aging test of the element (3) was 60 hours at an initial luminance of lOOOOcdZm 2 .
- the temperature dependence of the PL intensity of the devices (1) to (3) was measured.
- the temperature dependence of the PL intensity of the single-layer film of the light-emitting materials A and B was also measured. The results are shown below.
- the firing temperatures for forming the single-layer films of the light-emitting materials A and B were 150 ° C (light-emitting material A) and 150 ° C (light-emitting material B), respectively.
- FIG. 2 is a graph showing the temperature dependence of the PL intensity of the single-layer film made of the devices (1) and (2) and the light emitting material A. Since it is difficult to compare the PL intensity based on the absolute value, the PL intensity at room temperature (300K) should be standardized to 1 and illustrated! /
- the PL intensity of the single-layer film made of the luminescent material A increases with decreasing temperature, and the PL intensity at 5 K is 1.24 times the PL intensity at 300 K.
- the PL intensity at 5K decreases with decreasing temperature, and the PL intensity at 5K is weaker than the PL intensity at 300K.
- k is a luminescence rate constant
- ⁇ is a fluorescence lifetime
- k is a non-luminescence inactivation rate constant
- k is a rate constant of internal intersystem crossing.
- the PL intensity that is, the quantum yield ⁇ is proportional to the fluorescence lifetime ⁇ .
- k and k have no temperature dependence.
- nr is a heat-inactivating component and becomes smaller at low temperatures. Therefore, the value of the fluorescence lifetime ⁇ is increased by the low-temperature irradiation, and the quantum yield ⁇ is increased, and as a result, the PL intensity is increased.
- the PL strength decreases as the temperature decreases. This is because, in the devices (1) and (2), as shown in FIG. 1, the light emitting layer 4 formed by the light emitting layer 4 being sandwiched between the hole transport material 3 and the cathode 5 and the hole transport material It is considered that the exciton generated by the excitation light is quenched (quenched) at the interface with 3 and the interface between the light emitting layer 4 and the cathode 5.
- the quenched site may be simply a non-luminescent hole transporting material 3 or a cathode 5, or may be a non-luminescent state newly generated by the interaction between interfaces.
- Quenching of the exciton is caused by the exciton diffusing to the quenched site generated at the lamination interface and quenching.
- the diffusion mode of excitons here is considered to be resonance type diffusion (Forster type migration) or exciton diffusion (delocalization of excitons in the molecular chain or between molecules). If the decrease in PL intensity generated in this way has temperature dependence, the reason for the decrease in PL intensity associated with the low temperature of the organic EL element is that the exciton diffusion length is increased due to the low temperature. And the number of quenchinda sites are likely to increase.
- the difference in the decrease in PL strength of the organic EL element is caused by the interaction at the interface between the light emitting layer 4 and the hole transport material 3 and the interface between the light emitting layer 4 and the cathode 5 caused by the lamination, Exciton diffusion It is thought to be caused by differences in characteristics.
- the element (1) having a longer luminance half-life has a larger decrease in PL intensity from 300K to 5K. This indicates that the device (1) has larger interface interaction and exciton diffusion characteristics! /
- FIG. 3 shows the temperature dependence of the PL intensity of the single-layer film made of the element (3) and the light-emitting material B, as in the elements (1) and (2).
- the PL intensity at 5K is larger than that at 300K, as in the case of the single-layer film having the light-emitting material A force.
- element (3) differs from elements (1) and (2) in that the PL intensity at 5K is greater than the PL intensity at 300K. This is because the interaction between the interface between the light emitting material 4 and the hole transporting material 3 and the interface between the light emitting layer 4 and the cathode 5 is weaker in the element (3) than in the elements (1) and (2). This suggests that the system is a system and that exciton diffusion is likely to occur.
- Such an element (3) has a luminance half-life that is much shorter than the elements (1) and (2).
- FIG. 4 shows the relationship between the reduction rate of the PL intensity of the organic EL element and the half-time of luminance of the organic EL element due to the low temperature from 300 K to 5 K.
- the PL intensity reduction rate in FIG. 4 is expressed by the following equation (4).
- a PL intensity reduction rate of greater than ⁇ means that the PL intensity of the organic EL element decreases with low temperature. This means that the PL intensity reduction rate is smaller than 0, which means that the PL intensity of the organic EL element increases with low temperature. From FIG. 4, it can be seen that the higher the rate of decrease in the PL strength of the organic EL device due to the decrease in temperature from 300K to 5K, the longer the device life.
- P L intensity reduction rate (%) ⁇ (PL intensity at 300 K)-1 (PL intensity at 5 K) ⁇ / (PL intensity at 300 K) X I 0 0 (4)
- FIG. 5 shows the relationship between the PL intensity ratio Y and the luminance half-life of the organic EL element.
- a PL intensity ratio of less than 1 means that a decrease in PL intensity due to the low-temperature shading of the organic EL device is smaller than that of the light-emitting material single-layer film.
- a value greater than 1 means that the decrease in PL strength due to the low temperature of the organic EL element is greater than that of the single-layer light emitting material film. From FIG. 5, it can be seen that the smaller the PL intensity ratio Y, the longer the device life.
- Some light-emitting materials have a large degree of heat deactivation in the photoexcited state.
- the PL intensity may increase as the temperature decreases from 300K to 5K. There is. In such a case, it is not possible to estimate the degree of the decrease in PL intensity due to the device, but it is possible to estimate the degree of the decrease in PL intensity due to the device by comparing with a single-layer film of the luminescent material. As a result, the element life can be estimated.
- FIGS. 4 and 5 clearly show the relationship between the temperature dependence of the PL intensity of various devices and the device lifetime. From these results, it was a component that it was possible to obtain an element having excellent lifetime characteristics by using an element configuration in which the temperature dependence of PL intensity was large V.
- FIG. 6 shows a fluorescence intensity decay curve as shown in FIG. 6
- This attenuation curve was a component of the fact that there were two types of components that formed the PL intensity of element (1).
- a fluorescence decay curve of a fluorescent compound used in an organic EL device or the like shows an exponential decay characteristic as shown in FIG. 7, and the fluorescent component is often a single component.
- FIG. 7 shows the fluorescence decay characteristics of the luminescent material A used this time in a solution state.
- the attenuation characteristic of a single fluorescent component is represented by the following equation (5).
- I PL intensity
- A the initial PL intensity (constant) of the fluorescent component, and thus the fluorescence lifetime.
- the fluorescent component usually shows a linear attenuation characteristic.
- the decay characteristic is curved as shown in Fig. 6, it cannot be explained by a single fluorescent component, but is composed of multiple fluorescent components having different fluorescent lifetimes.
- the fluorescence decay characteristic is simply represented by the following equation (6), and the PL intensity I is a plurality of values. This is considered to be the sum of the PL intensity of the fluorescent component.
- A, B, etc. represent the initial PL intensity (constant) of each fluorescent component, and ⁇ , ⁇ , etc.
- the luminescent material A used in Example 2 had only one fluorescent component in the solution state as shown in FIG. 7, it was in the thin film state, that is, as shown in FIG. 6, in the device. Will have two types of fluorescent components. This is because, in the solution state, the luminescent material spreads in the solution and emits fluorescence by a single luminescent mechanism, but in the thin film state, the luminescent material is more aggregated in the film, so that it is contained in the constituent molecules or molecules. It is thought that the interaction between the two became large, resulting in two types of light emission mechanisms.
- the luminescent material B used in Comparative Example 1 had a single fluorescent component not only in a solution state but also in a thin film state (element (3)), and the element life was extremely short. Therefore, it has been found that an element having a plurality of fluorescent components in an element state can provide an element having an excellent element life.
- the element (2) also has two kinds of fluorescent components.
- Element (1) two fluorescent components which in the item (2), each fluorescence lifetime is a component and 7n Sec about components of about 2nse C.
- a fluorescent component having a fluorescence lifetime of 2 nsec is referred to as a fluorescent component 1
- a fluorescent component having a fluorescence lifetime of 7 nsec is referred to as a fluorescent component 2.
- the fluorescence decay curve of the device (1) obtained in FIG. 6 was separated into fluorescent components 1 and 2, and the temperature dependence of the PL intensity of each fluorescent component is shown in FIG.
- element (2) the fluorescence components 1 and 2 were separated from the fluorescence decay curve, and the temperature dependence of the PL intensity of each fluorescence component is shown in FIG.
- the element (1) it can be seen from FIG. 8 that the PL intensity at 5K is relatively reduced to about 0.46 for the fluorescent component 1 and to about 0.25 for the fluorescent component 2.
- element (2) it can be seen from FIG.
- the fluorescence intensity of the neutral fluorescent component 2 was relatively reduced to about 0.35, but the degree of the decrease was smaller than that of the device (1).
- the PL intensity of each fluorescent component at a cryogenic temperature (5K) is lower than the PL intensity at a normal temperature (300K). It can be seen that the device has a long device life. In addition, it can be seen that the greater the degree of the decrease in PL intensity due to the low temperature of each fluorescent component at room temperature and cryogenic temperature, the longer the lifetime and the device can be provided.
- a substrate having an insulating surface is preferable.
- a substrate formed of an inorganic material such as glass or quartz, a substrate formed of a plastic force such as polyethylene terephthalate, alumina, or the like is used.
- Ceramics A substrate formed, a substrate in which an insulator such as SiO or an organic insulating material is coated on a metal substrate such as aluminum-iron or iron, or gold.
- Substrates obtained by subjecting a surface of a metal substrate to an insulation siding treatment by a method such as anodizing or the like can be widely used.
- a switching element such as a thin film transistor (TFT) may be formed on the substrate 1.
- TFT thin film transistor
- a polysilicon TFT is formed by a low-temperature process, it is preferable to use a substrate that does not melt at a temperature of 500 ° C. or lower and does not cause distortion.
- a polysilicon TFT is formed by a high-temperature process, it is preferable to use a substrate that does not melt at a temperature of 1000 ° C. or less and does not cause distortion.
- the anode 2 and the cathode 5 can be formed using a conventionally known electrode material.
- Materials for the anode 2 for injecting holes into the organic layer 4 include metals having a high work function such as Au, Pt, and Ni; ITO, IDIXO ⁇ indium indium zinc oxide; In O (ZnO) ⁇ ,
- Examples include a transparent conductive material such as SnO.
- the cathode 5 for injecting electrons into the organic layer 4 includes a metal electrode in which a metal having a low work function such as CaZAl, Ce / AU Cs / AU BaZAl and a stable metal are laminated, a Ca: Al alloy, a Mg: Ag alloy, Metal electrode containing metal with low work function such as Li: A1 alloy, electrode combining insulating layer (thin film) such as LiF / AU LiF / Ca / AU BaF ZBaZAl and metal electrode
- the anode 2 and the cathode 5 can be formed by vapor deposition, electron beam (Electro A dry process such as an n Beam (EB) method, a molecular beam epitaxy (MBE) method, a sputtering method, or a wet process such as a spin coating method, a printing method, and an ink jet method can be used.
- electron beam Electro A dry process such as an n Beam (EB) method, a molecular beam epitaxy (MBE) method, a sputtering method, or a wet process such as a spin coating method, a printing method, and an ink jet method can be used.
- the light emitting layer 4 may have a single-layer structure or a multilayer structure.
- the light emitting layer 4 can be formed using a conventionally known organic light emitting material.
- the light emitting layer 4 can be formed by dissolving a light emitting material in a solvent to prepare an organic light emitting layer forming coating liquid as in the present embodiment, and using it to perform a wet process.
- the coating liquid for forming an organic light emitting layer is a solution containing at least one light emitting material, and may contain two or more light emitting materials.
- the solvent used in the coating liquid for forming the organic light emitting layer is not particularly limited as long as it can dissolve or disperse the light emitting material.
- the coating liquid for forming an organic light emitting layer may contain a resin for binding in addition to a light emitting material.
- a leveling agent, a light emission assisting agent, a charge injection transport material, an additive (Donor, acceptor, etc.) and a luminescent dopant examples include polycarbonate and polyester.
- the light emitting layer 4 may be formed by a dry process. The light emitting layer 4 formed by the dry process may also contain a light emitting assisting agent, a charge transporting material, an additive (donor, acceptor, etc.), a light emitting dopant, and the like.
- a conventionally known light emitting material for an organic EL element can be used, but it is not particularly limited to this. Specifically, a precursor of a low molecular light emitting material, a high molecular light emitting material, a high molecular light emitting material, or the like can be used.
- low molecular light emitting material examples include aromatic dimethylidene compounds such as 4,4,1-bis (2,2, diphenyl-biphenyl) -biphenyl (DPVBi), 5-methyl-2- [2- [4-1-1 Oxadiazole compounds such as (5-methyl-2-benzoxazolyl) phenyl] vinyl] benzoxazole, 3- (4-biphenyl-)-4-phenyl-5-t-butylphenyl — Triazole derivatives such as 1,2,4 triazole (TAZ), styrylbenzene compounds such as 1,4 bis (2-methylstyryl) benzene, thiopyrazinedioxide derivatives, benzoquinone derivatives, naphthoquinone derivatives, anthraquinone derivatives, Diphenoquinone derivatives, Examples include fluorescent organic materials such as a fluorenone derivative, fluorescent organic metal compounds such as an azomethine zinc complex, and (8-hydroxyquinolinato) aluminum
- polymer light emitting material for example, poly (2-decyloxy-1,4-phenylene) (DO-PPP), poly [2,5-bis [2- (N, N, N-triethylammonium) ethoxy]- 1,4-phenyl-alto-1,4-phenylene] dibromide (PPP—NEt 3+ ), poly [2- (2, -ethylhexyloxy)) 5-methoxy-1,4-phenylene- Len] (MEH-PPV), poly [5-methoxy-1- (2propanoxysulfoxide) -1,4 phen-lenvylene] (MPS-PPV), poly [2,5 bis (hexyloxy) Fluorescent organometallic compounds such as 1,4-phenylene- (1-cyano-virene)] (CN-PPV) and poly (9,9-dioctylfluorene) (PDAF).
- the precursor of the polymer light emitting material include a
- the hole transport layer 3 can be formed by a wet process using a coating liquid for forming a hole transport layer in which at least one type of hole transport material is dissolved in a solvent.
- the coating liquid for forming a hole transport layer may contain two or more kinds of charge injection / transport materials. Further, the coating liquid for forming a hole transport layer may contain a resin for binding or may contain a leveling agent, an additive (donor, axceptor, etc.) in addition to the resin.
- the binder resin for example, polycarbonate, polyester, or the like can be used.
- the solvent used in the hole transport layer forming coating liquid is not particularly limited as long as it can dissolve or disperse the hole transport material.
- the hole transport layer 3 may be formed by a dry process.
- the hole transport layer 3 formed by the dry process may also contain additives (donor, receptor, etc.).
- an inorganic P-type semiconductor material a vorphyrin compound, N, N, 1-bis (3-methylphenyl) N, N, 1-bis (phenyl) -1-benzidine (TPD), N, N, 1-di (naphthalene-1-yl) N, N, 1-diphenyl Aromatic tertiary amine compounds such as benzidine (NPD), low molecular weight materials such as hydrazonyi conjugates, quinacridone compounds, styrylamine conjugates, polyaline (PANI), 3,4 polyethylene dioxytio Fen Z Polymer materials such as polystyrene sulfonate (PEDOTZPSS), poly [triphenylamine derivative] (Poly-TPD), polybutyl rubazole (PVCz), and poly (p-phenylene-lene) precursor (Pre-PPV) And a polymer
- Embodiment 2 according to the present invention will be described with reference to FIG.
- the inspection device for an organic EL device of the present embodiment is capable of estimating the life of the device without performing an aging test and discriminating a non-defective product. It can also be used to determine optimum conditions such as process conditions and materials.
- the inspection apparatus includes an excitation light source 6 that irradiates a test element 7 with excitation light, a detector 9 that detects fluorescence emitted from the test element 7, a test element 7, and its surroundings.
- a temperature control device 8 that can control the temperature of the laser beam and a data storage processing device 10 that can record and compare the detected PL intensity are provided. Note that the arrows in FIG. 10 schematically show the optical paths of the excitation light and the fluorescence.
- the excitation light source 6 is not particularly limited as long as it can excite the light emitting material used in the element.
- a light source that emits a laser beam having a center wavelength at 325, 337, or 365 nm For example, a light source device that extracts and emits light having an excitation wavelength that is optimal for a light-emitting material by using a monochromator with white light is used.
- a nitrogen laser-excited dye laser center wavelength: 337 nm was used.
- the detector 9 is not particularly limited as long as it can monitor the PL intensity of the test element 7, and for example, a device that monitors a photocurrent with a photodiode, or a device that measures a fluorescence spectrum with a spectroscope and uses the area thereof.
- a device for monitoring the PL intensity may be used.
- a system that includes a streak scope and a spectroscope and measures the fluorescence energy within a certain time is used.
- the temperature control device 8 a cooling unit, a heater, a control device that controls the output of the cooling unit and the heater to control the temperature to an arbitrary temperature, and the like are used.
- a control device using a cryostat is suitably used.
- the force measured for the PL intensity at room temperature and at a very low temperature using a cryostat changes in the PL intensity closer to room temperature, If it clearly appears, for example, a liquid nitrogen cooling unit can be used to compare the PL intensity between room temperature and liquid nitrogen temperature (about 70K).
- an inspection for the life characteristics of the organic EL element was performed as follows using an inspection apparatus for an organic EL element having the above-described configuration.
- the characteristics shown in Fig. 4 were stored in the inspection device in advance.
- the test sample 7 was injected there, the PL intensity at room temperature (300K) and the PL intensity at 5K were measured, and the intensity ratio was calculated by the data storage processor 10.
- the element life of the test sample 7 was estimated by comparing the value of the intensity ratio obtained in this manner with the characteristics in FIG. An aging test was actually performed on this test sample 7 to confirm the results. As a result, almost the same results as the life estimations calculated by this test device were obtained.
- the organic EL device inspection apparatus of the present embodiment it is not necessary to perform an aging test, so that the device life can be easily estimated in a short time without deteriorating the device. Further, the organic EL element after the inspection can be used as a practical product as it is because the element characteristics are not impaired by the inspection.
- the following test was performed to find the optimum conditions of the element configuration of the organic EL element using the inspection device for the organic EL element having the above-described configuration.
- an organic EL device using a new light-emitting material C an element having a structure in which ITO, PED III, light-emitting material C and a cathode are sequentially laminated, the film thickness of PEDOT, the light-emitting material C
- the device was manufactured by changing the film thickness and the cathode material under various conditions. Among them, in order to find the condition with the best device life, the life of the device fabricated under each condition was estimated using an inspection device.
- FIG. 1 is a cross-sectional view schematically showing a cross-sectional configuration of an organic electroluminescence element according to Embodiment 1.
- FIG. 2 is a diagram for explaining the temperature dependence of the photoluminescence intensity of the organic electroluminescent device according to Examples 1 and 2 of the present invention and the light emitting layer (single-layer film of the light emitting material) constituting the organic electroluminescent device. .
- FIG. 3 is a diagram illustrating the temperature dependence of the photoluminescence intensity of the organic electroluminescent element according to Comparative Example 1 and the light emitting layer (light emitting material single layer film) constituting the same.
- FIG. 4 is a view for explaining the relationship between the reduction rate of the photoluminescence intensity of the organic electroluminescence element and the half-life of luminance.
- FIG. 5 is a diagram for explaining a relationship between a photoluminescence intensity ratio Y and a half-life of luminance of an organic electroluminescence element.
- FIG. 6 is a diagram showing a fluorescence decay characteristic of a device (1) according to Example 1 of the present invention.
- FIG. 7 is a diagram showing a fluorescence decay characteristic of a light-emitting material A according to Examples 1 and 2 of the present invention in a solution state.
- FIG. 8 is a diagram for explaining the temperature dependence of the photoluminescence intensity of the device (1) according to Example 1 of the present invention and the fluorescent components 1 and 2 thereof.
- FIG. 9 is a diagram for explaining the temperature dependence of the photoluminescence intensity of the device (2) according to Example 2 of the present invention and the fluorescent components 1 and 2 thereof.
- FIG. 10 is a diagram schematically showing a configuration of an inspection device for an organic electroluminescence element according to a second embodiment of the present invention.
- Temperature control device Detector
Abstract
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JP2006514671A JPWO2005122702A1 (ja) | 2004-06-16 | 2005-05-16 | 有機エレクトロルミネセンス素子、その検査装置及び検査方法 |
US11/570,714 US7595587B2 (en) | 2004-06-16 | 2005-05-16 | Organic electroluminescent element exhibiting temperature-dependent photoluminescence intensity |
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WO2005122702A3 (ja) | 2006-09-21 |
JPWO2005122702A1 (ja) | 2008-04-10 |
US20070298279A1 (en) | 2007-12-27 |
KR100839732B1 (ko) | 2008-06-19 |
US7595587B2 (en) | 2009-09-29 |
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