WO2013157058A1 - 有機el素子 - Google Patents
有機el素子 Download PDFInfo
- Publication number
- WO2013157058A1 WO2013157058A1 PCT/JP2012/005590 JP2012005590W WO2013157058A1 WO 2013157058 A1 WO2013157058 A1 WO 2013157058A1 JP 2012005590 W JP2012005590 W JP 2012005590W WO 2013157058 A1 WO2013157058 A1 WO 2013157058A1
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- WIPO (PCT)
- Prior art keywords
- oxide
- organic
- hole injection
- layer
- injection layer
- Prior art date
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Classifications
-
- 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]
- H10K50/17—Carrier injection layers
-
- 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
-
- 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 electroluminescent element (hereinafter referred to as “organic EL element”) which is an electroluminescent element.
- the organic EL element is a current-driven light emitting element and has a structure in which a functional layer containing an organic material is interposed between an electrode pair composed of an anode and a cathode.
- the functional layer includes a light emitting layer, a buffer layer, and the like.
- a hole injection layer for injecting holes may be interposed between the functional layer and the anode.
- the driving of the organic EL element utilizes an electroluminescence phenomenon generated by recombination of holes injected from the anode into the functional layer and electrons injected from the cathode into the functional layer by applying a voltage between the electrode pair.
- Organic EL elements are self-luminous, have high visibility, and have excellent characteristics such as impact resistance because they are completely solid elements, so their use as light-emitting elements and light sources in various display devices is attracting attention. Has been.
- Organic EL elements are roughly classified into two types depending on the type of material used for the functional layer and the formation method.
- the first type is a vapor deposition type organic EL element in which a low molecular material is mainly used as a functional layer material and is formed by using a vacuum process such as a vapor deposition method.
- As the second type a coating type organic EL element formed by using a high molecular weight material or a low molecular weight material having a good thin film formability as a functional layer material and using a wet process such as an ink jet method or a gravure printing method. It is.
- the vapor deposition type organic EL element which is the first type has been developed in advance for reasons such as high luminous efficiency of the luminescent material and long driving life. Practical use has begun in displays and small televisions.
- the coating type organic EL element which is the second type is effective for realizing a large-sized organic EL panel, and is also being developed.
- Such R & D targets include a hole injection layer that is interposed between the functional layer and the anode and greatly contributes to improvement in luminous efficiency.
- a hole injection layer using an organic material such as copper phthalocyanine or PEDOT (conductive polymer), but in recent years, a metal oxide such as nickel oxide or tungsten oxide is used. Attempts have been made to form a hole injection layer (see Patent Documents 1 and 2).
- Non-Patent Documents 1 and 2 improvement in hole injection efficiency and luminance has been reported (see Non-Patent Documents 1 and 2), and in particular, nickel oxide. It has been reported that a good luminance can be obtained by increasing the composition ratio of oxygen in the hole injection layer made of and thus increasing the ratio of Ni 3+ in the hole injection layer (Patent Document 1, Non-Patent Document 1). (See Patent Document 3).
- a coating solution containing an organic functional material is applied on the hole injection layer made of nickel oxide, and then heat treatment is performed.
- This heat treatment is for removing the solvent by volatilization.
- the conditions of the heat treatment depend on the solvent used, but for example, the heating is performed in a nitrogen atmosphere by heating to a temperature at which the organic functional material does not change or decompose, generally about 100 to tens of degrees [° C.]. Is called.
- the hole injection layer made of nickel oxide is also heated at the temperature and the atmosphere.
- the present invention has been made to solve the above-described problems, and can provide a high hole injection efficiency even when subjected to heat treatment while including a hole injection layer containing a p-type metal oxide. It aims at providing the organic EL element which can be performed.
- an organic EL device includes an anode and a cathode that are arranged to face each other with a space therebetween, and an organic material, and is interposed between the anode and the cathode. And a hole injection layer having a function of injecting holes into the functional layer and interposed between the anode and the functional layer, wherein the hole injection layer is a first oxide. And a mixed layer containing the second oxide.
- the first oxide is a p-type metal oxide
- the element included in the composition of the second oxide has a maximum valence. Both the first state and the second state that takes a valence less than the maximum valence are thermally stable, and the second state is more thermally stable than the first state.
- the second oxide contained in the hole injection layer includes the element in the first state.
- the hole injection layer is configured as a mixed layer containing a first oxide (p-type metal oxide) and a second oxide.
- the 2nd oxide shall contain the element which can take the above two valence states.
- the valence state effective for hole injection in the hole injection layer is good even in the heat treatment in the functional layer formation step of the coating type organic EL element with the above structure. And good hole injection efficiency can be maintained. Thereby, manufacture of the organic EL element which can endure the mass production process of an organic EL panel can be performed.
- An organic EL device includes an anode and a cathode that are arranged to face each other with a space therebetween, a functional layer that includes an organic material, and is interposed between the anode and the cathode, and the function
- a hole injection layer having a function of injecting holes into the layer and interposed between the anode and the functional layer, wherein the hole injection layer includes a first oxide and a second oxide. It is a mixed layer containing.
- the first oxide is a p-type metal oxide
- the element included in the composition of the second oxide has a maximum valence. Both the first state and the second state that takes a valence less than the maximum valence are thermally stable, and the second state is more thermally stable than the first state.
- the second oxide contained in the hole injection layer includes the element in the first state.
- thermally stable means that the valence can exist without changing on average.
- the second state is more thermally stable than the first state” means that the second state can maintain the valence on average even in a higher temperature environment.
- the “element” is specifically at least one of elements other than oxygen constituting the oxide.
- the valence state effective for hole injection in the hole injection layer is well maintained even in the heat treatment in the formation process of the functional layer of the coating type organic EL element. And good hole injection efficiency can be maintained. Thereby, manufacture of the organic EL element which can endure the mass production process of an organic EL panel can be performed.
- the organic EL element according to one embodiment of the present invention can have a difference between the maximum valence and the valence less than 2 in the elements contained in the composition of the second oxide. Due to this difference in valence, the valence state effective for hole injection can be favorably maintained for the element in the first oxide during the heat treatment.
- the element contained in the composition of the second oxide is an element in which an electron pair is formed in the outermost shell s orbital most stably. Can do. In other words, it is an element that exhibits an inert electron pair effect.
- the element contained in the composition of the second oxide can be specifically Tl, Pb, Bi, Se, In, Sn, Sb. .
- the organic EL device according to one embodiment of the present invention can include at least one element of Ni, Cu, Co, Fe, Cr, and Mn in the composition of the first oxide.
- the element included in the composition of the first oxide can have a higher ionization tendency than the element included in the composition of the second oxide.
- FIG. 1 is a schematic cross-sectional view showing a configuration of an organic EL element 1 according to the present embodiment.
- the organic EL element 1 is a coating type organic EL element manufactured by applying a functional layer by a wet process. Specifically, as shown in FIG. 1, in the organic EL element 1, an anode 11 and a hole injection layer 12 are sequentially stacked on one main surface of a substrate 10. A bank 13 is formed on the hole injection layer 12 so that a part of the main surface is exposed.
- a buffer layer 14 and a light emitting layer 15 are sequentially stacked in an opening formed by the surrounding of the bank 13, and a cathode 16 composed of a barium layer 16a and an aluminum layer 16b is stacked thereon.
- the anode injection layer 12 and various functional layers that include an organic material and have a predetermined function are stacked on each other.
- 11 and a cathode 16 is interposed between the electrode pair.
- a DC power source 17 is connected to the anode 11 and the cathode 16 for the organic EL element 1.
- the anode 11 is composed of, for example, an ITO thin film having a thickness of 50 [nm].
- the hole injection layer 12 is made of, for example, a mixed layer of nickel oxide and bismuth oxide having a thickness of 7.5 [nm].
- the hole injection layer 12 is preferably composed of only elements of nickel, bismuth, and oxygen as much as possible, but may contain a trace amount of impurities to such an extent that it can be mixed at a normal level.
- the hole injection layer 12 is formed under specific film formation conditions described later. This includes Ni 3+ and Bi 5+ which is the maximum valence of bismuth. With this configuration, in the organic EL element 1 according to the present embodiment, Ni 3+ in the hole injection layer 12 can be satisfactorily maintained even after the bank 13, the buffer layer 14, and the light emitting layer 15 are baked.
- a bank 13 made of an insulating organic material (for example, an acrylic resin, a polyimide resin, a novolac type phenol resin, etc.) has a stripe structure or a cross structure having a certain trapezoidal cross section. It is formed to make. Functional layers (buffer layer 14 and light emitting layer 15) made of an organic material and formed by a wet process are formed in an opening formed by the bank 13.
- an insulating organic material for example, an acrylic resin, a polyimide resin, a novolac type phenol resin, etc.
- bank 13 is not an essential component of the present invention, and is unnecessary when the organic EL element 1 is used alone.
- the buffer layer 14 may be, for example, TFB (poly (9,9-di-n-octylfluorene-alt- (1,4-phenylene-((4-sec- butylphenyl) imino) -1,4-phenylene)).
- the light emitting layer 15 is made of, for example, F8BT (poly (9, 9-di-n-octylfluorene-alt-benzothiazole)) which is an organic polymer having a thickness of 70 [nm].
- F8BT poly (9, 9-di-n-octylfluorene-alt-benzothiazole)
- the constituent material of the light-emitting layer 15 is not limited to the above-described materials, and can be configured to include other known organic materials.
- the buffer layer 14 and the light emitting layer 15 are functional layers. However, either one of these layers, a hole transport layer that transports holes, or the like, or two layers thereof. A combination of the above or all layers can also be indicated.
- the hole injection layer is targeted, but the organic EL element has layers that perform the required functions such as the hole transport layer and the light emitting layer described above in addition to the hole injection layer.
- the functional layer refers to a layer necessary for the organic EL element other than the hole injection layer which is an object of the present invention.
- the cathode 16 is configured, for example, by laminating a barium layer 16a having a thickness of 5 [nm] and an aluminum layer 16b having a thickness of 100 [nm] in this order.
- the DC power source 17 is connected to the anode 11 and the cathode 16, and power is supplied to the organic EL element 1 from the outside.
- the substrate 10 is, for example, alkali-free glass, soda glass, non-fluorescent glass, phosphate glass, borate glass, quartz, acrylic resin, styrene resin, polycarbonate resin, epoxy resin, polyethylene, polyester, silicone resin. Or an insulating material such as alumina.
- the hole injection layer 12 made of a mixed layer of nickel oxide and bismuth oxide contains Ni 3+ and Bi 5+ which is the maximum valence of bismuth.
- the substrate 10 is placed in the chamber of the sputter deposition apparatus. Then, a predetermined sputtering gas is introduced into the chamber, and the anode 11 made of an ITO film having a thickness of 50 [nm] is formed by, for example, reactive sputtering.
- the hole injection layer 12 is formed, but it is preferable to form the film using a sputtering method.
- a sputtering method when the structure of this embodiment is applied to a large-sized organic EL panel that requires film formation of a large area, there is a possibility that unevenness may occur in film thickness or the like when film formation is performed using an evaporation method or the like.
- the film is formed by sputtering, it is easy to avoid such film formation unevenness.
- NiO nickel oxide
- Bi 2 O 3 dibismuth trioxide
- film formation is performed using a reactive sputtering method.
- oxygen gas is introduced into the chamber together with argon gas, so that Ni 3+ is formed by excess oxygen in nickel oxide, and oxidation is further promoted in bismuth oxide to achieve the most stable value.
- Bi 5+ which is the maximum and stable valence is formed together with Bi 3+ which is a number.
- stable means that the valence can exist on average at normal temperature and atmospheric pressure or in a nitrogen atmosphere, and the heat treatment during the manufacturing process of the organic EL element 1 is performed. Sometimes it may change.
- a photosensitive resist material for example, a photosensitive resist material, preferably a photoresist material containing a fluorine-based material is prepared.
- This bank material is uniformly applied on the hole injection layer 12 and prebaked, and then a mask having an opening having a predetermined shape (a bank pattern to be formed) is overlaid. Then, after exposure from above the mask, uncured excess bank material is washed out with a developer. Finally, the bank 13 is completed by washing with pure water.
- a composition ink containing an amine-based organic molecular material on the surface of the hole injection layer 12 exposed in the opening surrounded by the bank 13 by, for example, a wet process using an inkjet method or a gravure printing method.
- the solvent is xylene
- the solvent is volatilized and removed by heat treatment at 130 [° C.] for 30 minutes in a nitrogen atmosphere.
- the buffer layer 14 is formed.
- a composition ink containing an organic light-emitting material (for example, the solvent is xylene) is dropped onto the surface of the buffer layer 14 in the same manner as described above, and heated at 200 [° C.] for 10 minutes in a nitrogen atmosphere. By the treatment, the solvent is removed by volatilization. Thereby, the light emitting layer 15 is formed.
- an organic light-emitting material for example, the solvent is xylene
- the formation method of the buffer layer 14 and the light emitting layer 15 is not limited to this, Well-known methods, such as methods other than an inkjet method and a gravure printing method, for example, a dispenser method, a nozzle coat method, a spin coat method, intaglio printing, letterpress printing, etc.
- the ink may be dropped and applied by a method.
- a barium layer 16a and an aluminum layer 16b are sequentially formed on the surface of the light emitting layer 15 by using, for example, a vacuum deposition method. Thereby, the cathode 16 is formed.
- a sealing layer is further provided in the surface of the cathode 16, or the whole organic EL element 1 is made.
- a sealing can that is spatially isolated from the outside can also be provided.
- the sealing layer can be formed using, for example, a material such as SiN (silicon nitride) or SiON (silicon oxynitride), and is provided so as to internally seal the organic EL element 1.
- a sealing can When using a sealing can, it can be formed using, for example, the same material as the substrate 10 as the sealing can, and a getter that adsorbs moisture or the like can be provided in the sealed space.
- the organic EL element 1 is completed through the above steps.
- Table 1 shows the sputtering film forming conditions for each sample.
- the input power, total pressure, and film thickness are 200 [W], 8 [Pa], and 7.5 [nm] for all samples.
- the sample numbers shown in Table 1 are used. Alternatively, use the sample name.
- X-ray photoelectron spectroscopy (XPS) measurement was performed on each prepared sample.
- the XPS spectrum generally reflects the elemental composition from the surface of the measurement object to the depth number [nm], and the electronic state such as the bonding state and valence.
- FIG. 1-No. 3 is a spectrum of Ni 2p in each of 3; The peak indicated by arrow A in the figure is attributed to Ni 2+, and the shoulder structure indicated by arrow B is attributed to Ni 3+ .
- FIG. 2 and no. 3 is a spectrum of Bi 4f in each of 3; The two main peaks indicated by arrow C in the figure are attributed to Bi 3+, and the two shoulder structures indicated by arrow D are attributed to Bi 5+ .
- FIG. 1-No. 3 is a spectrum of O 1s in each of 3; Sample No. indicated by arrow E in the figure. 2 “Bi—NiO film” and sample no.
- the peak on the high bond energy side of “O-increased Bi—NiO film” of No. 3 indicates the existence of a bond state having higher covalent bond than Bi—O bond and Ni—O bond, The O 2 molecule is considered.
- the presence of Bi 5+ in the mixed film of nickel oxide and bismuth oxide may increase Ni 3+ when Bi 5+ changes to Bi 3+ which is more thermally stable. I understand.
- the hole injection layer 12 made of a mixed layer of nickel oxide and bismuth oxide provided in the organic EL element 1 according to the above embodiment is heated in the functional layer forming step. Even after the treatment, since Ni 3+ is held well, a good hole injection efficiency can be maintained.
- the change from Bi 5+ to Bi 3+ progresses as the temperature rises. Will go in the direction. Therefore, the configuration of the above embodiment has an effect of supplying Ni 3+ originally lost by the heat treatment.
- the decrease in Ni 3+ can be suppressed even after the heat treatment of the bank 13, the buffer layer 14, and the light emitting layer 15.
- Low voltage driving can be realized by ensuring a high hole injection efficiency.
- the fabricated hole-only element 2 is formed with an anode 21 made of an ITO thin film having a thickness of 50 [nm] on a substrate 20, and further, an oxidation is formed on the anode 21.
- a hole injection layer 22 having a thickness of 7.5 [nm] made of a mixed layer of nickel and bismuth oxide, a buffer layer 24 having a thickness of 20 [nm] made of TFB which is an amine organic polymer, and F8BT being an organic polymer.
- the light emitting layer 25 having a thickness of 70 [nm] and the cathode 26 having a thickness of 100 [nm] made of Au (gold) are sequentially stacked.
- the hole-only element 2 for evaluation is mainly characterized in that the cathode 16 is replaced with a cathode 26 made of Au (gold) with respect to the organic EL element 1 according to the embodiment shown in FIG. It is an element.
- the buffer layer 24 and the light emitting layer 25 have undergone respective heat treatments. Since it is an evaluation device, the bank is omitted.
- the produced Hall-only element 2 was connected to a DC power source 27 and a voltage was applied. Then, the applied voltage was changed, and the current value that flowed according to the voltage value was converted to a value (current density) per unit area of the element 2.
- the “drive voltage” is an applied voltage at a current density of 10 [mA / cm 2 ].
- Ni 3+ in the hole injection layer 22 increases, in other words, if the nickel oxide becomes p-type and p-type carriers increase in the hole injection layer 22, the interface between the anode 21 and the hole injection layer 22. Is closer to ohmic connection, and the conductivity of the hole injection layer 22 itself is also improved.
- the hole injection barrier between the hole injection layer 22 and the buffer layer 24 is also reduced.
- the overall hole injection efficiency of the hole-only element 2 is improved and appears as a decrease in drive voltage.
- FIG. 6 shows current density-applied voltage curves of two types of hole-only elements 2 in which the configuration of the hole injection layer 22 is changed.
- the vertical axis in the figure is current density [mA / cm 2 ], and the horizontal axis is applied voltage [V].
- the hole-only device 2 that employs the hole injection layer 22 made of “NiO film” is referred to as “NiO-HOD”, and the hole-only device 2 that employs the hole injection layer 22 made of “O-increased Bi—NiO film” is “ O increase Bi-NiO-HOD ".
- Bi-increased Bi-NiO-HOD has a lower driving voltage and a faster rise of the current density-applied voltage curve than “NiO-HOD”. That is, “O increased Bi—NiO—HOD” has a higher current density at a lower applied voltage than “NiO—HOD”.
- the hole-only element 2 is the organic EL element 1 according to the embodiment shown in FIG. It is the same composition as. Therefore, the effect of promoting the formation of Ni 3+ by Bi 5+ in the hole injection layer 12 in the organic EL element 1 on the hole injection efficiency is essentially the same as that of the hole injection layer 22 of the hole-only element 2.
- a mixed layer of nickel oxide and bismuth oxide is used as the hole injection layer, but the present invention is not limited to this combination.
- Pb, Tl, In, Sn, and Sb are examples of elements that are stable at the maximum valence and less than that, such as Bi. It is known that these elements are most stable when an electron pair is formed in the outermost shell s orbital (inert electron pair effect).
- the p-type metal oxide may contain at least one of Ni, Cu, Co, Fe, Cr, and Mn as a constituent element.
- the element of the oxide of the element in which the maximum valence and the valence less than that are stable and the smaller valence is more stable may have a higher ionization tendency.
- the oxidation of the metal element of the p-type metal oxide (promotion of p-type conversion) due to the change from the maximum valence state to the most stable valence state of the former element becomes more effective, and higher hole injection Efficiency can be expected.
- the mixed layer that is the hole injection layer may be mixed at the atomic level or may be phase-separated.
- a mixed layer of nickel oxide and bismuth oxide it may be in the form of a Ni—Bi—O compound or glass in which Ni atoms and Bi atoms are close to each other, and NiO, Bi 2 O 3 , Bi 2 O 5, etc.
- the grains may be separated into grains. In the latter case, an ionic reaction can occur between Ni 3+ and Bi 5+ that are in contact with each other at the grain boundary.
- the present invention is useful for realizing various display panels including a large screen television and organic EL elements that are driven at a low voltage in a wide luminance range from low luminance to high luminance as various light sources.
- Organic EL element Hall-only element 10 20. Substrate 11, 21. Anodes 12, 22. Hole injection layer 13. Banks 14, 24. Buffer layers 15, 25. Light emitting layers 16, 26. Cathode 16a. Barium layer 16b. Aluminum layers 17, 27. DC power supply
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Abstract
Description
本発明の一態様に係る有機EL素子は、互いに間隔をあけて対向配置された陽極および陰極と、有機材料を含んでなり、陽極と陰極との間に介挿された機能層と、当該機能層にホールを注入する機能を有し、陽極と機能層との間に介挿されたホール注入層と、を備え、当該ホール注入層は、第1の酸化物と第2の酸化物とを含有する混合層である。そして、本発明の一態様に係る有機EL素子では、第1の酸化物がp型の金属酸化物であり、第2の酸化物は、その組成中に含まれる元素が、最大価数を取る第1状態と、最大価数よりも少ない価数を取る第2状態の何れにおいても熱的に安定であり、且つ、第2状態が第1状態よりも熱的に安定である。さらに、ホール注入層に含有される第2の酸化物は、第1状態で当該元素を含む、ことを特徴とする。
以下、本発明の実施の形態に係る有機EL素子1の構成を説明し、続いて各性能確認実験の結果と考察を述べる。
図1は、本実施の形態に係る有機EL素子1の構成を示す模式的な断面図である。
陽極11は、例えば、厚さ50[nm]のITO薄膜で構成されている。
ホール注入層12は、例えば、厚さ7.5[nm]の酸化ニッケルと酸化ビスマスとの混合層からなる。
ホール注入層12の表面の一部には、絶縁性の有機材料(例えばアクリル系樹脂、ポリイミド系樹脂、ノボラック型フェノール樹脂など)からなるバンク13が、一定の台形断面を持つストライプ構造または井桁構造をなすように形成されている。有機材料からなり、ウェットプロセスにより形成される機能層(バッファ層14、発光層15)は、バンク13の囲繞により構成された開口部内に形成される。
バッファ層14は、例えば、厚さ20[nm]のアミン系有機高分子であるTFB(poly(9、9-di-n-octylfluorene-alt-(1、4-phenylene-((4-sec-butylphenyl)imino)-1、4-phenylene))で構成される。
発光層15は、例えば、厚さ70[nm]の有機高分子であるF8BT(poly(9、9-di-n-octylfluorene-alt-benzothiadiazole))で構成される。しかしながら、発光層15の構成材料については、上記材料に限定されず、他の公知の有機材料を含むように構成することが可能である。例えば、特開平5-163488号公報に記載のオキシノイド化合物、ペリレン化合物、クマリン化合物、アザクマリン化合物、オキサゾール化合物、オキサジアゾール化合物、ペリノン化合物、ピロロピロール化合物、ナフタレン化合物、アントラセン化合物、フルオレン化合物、フルオランテン化合物、テトラセン化合物、ピレン化合物、コロネン化合物、キノロン化合物およびアザキノロン化合物、ピラゾリン誘導体およびピラゾロン誘導体、ローダミン化合物、クリセン化合物、フェナントレン化合物、シクロペンタジエン化合物、スチルベン化合物、ジフェニルキノン化合物、スチリル化合物、ブタジエン化合物、ジシアノメチレンピラン化合物、ジシアノメチレンチオピラン化合物、フルオレセイン化合物、ピリリウム化合物、チアピリリウム化合物、セレナピリリウム化合物、テルロピリリウム化合物、芳香族アルダジエン化合物、オリゴフェニレン化合物、チオキサンテン化合物、アンスラセン化合物、シアニン化合物、アクリジン化合物、8-ヒドロキシキノリン化合物の金属錯体、2-ビピリジン化合物の金属錯体、シッフ塩とIII族金属との錯体、オキシン金属錯体、希土類錯体等の蛍光物質等を挙げることができる。
本実施の形態では、上述のように、バッファ層14と発光層15とが機能層であるとしたが、これらの層、およびホールを輸送するホール輸送層などのいずれか、もしくはそれらの2層以上の組み合わせ、または全ての層を指すこともできる。本実施の形態では、ホール注入層を対象としているが、有機EL素子はホール注入層以外に上記したホール輸送層、発光層などのそれぞれ所要機能を果たす層が存在する。機能層とは、本発明の対象とするホール注入層以外の、有機EL素子に必要な層を指している。
陰極16は、例えば、厚さ5[nm]のバリウム層16aと、厚さ100[nm]のアルミニウム層16bをこの順に積層して構成されている。
以上の構成を持つ有機EL素子1では、酸化ニッケルと酸化ビスマスの混合層からなるホール注入層12において、Ni3+、および、ビスマスの最大価数であるBi5+を含む。これにより、後述するバンク13、バッファ層14、発光層15のベーク工程における加熱処理を経ても、Ni3+を良好に維持することができ、高いホール注入効率を維持することができる。
次に、有機EL素子1の全体的な製造方法を例示する。
〈酸化ニッケルに対する酸化ビスマスの効果について〉
上記実施の形態では、ホール注入層12を構成する酸化ニッケルと酸化ビスマスの混合層において、ビスマスの最大価数であるBi5+を存在させることにより、機能層の形成工程における加熱処理の実行によってもNi3+を良好に維持できる。このことは以下の実験で確認された。
使用機器:X線光電子分光装置 PHI5000 VersaProbe(アルバック・ファイ社製)
光源:Al Kα線
光電子出射角:基板法線方向
測定点間隔:0.1[eV]
[測定結果と考察]
測定結果のスペクトルを図2から図4に示す。なお、図2から図4の横軸は結合エネルギーであり、縦軸は各スペクトルの最大強度で規格化した光電子強度である。
[数2] Ni2+→Ni3++e-
このときBi-O結合が切られるため、Oが余り、O2として析出する。
[数3] 2Bi2O5+4NiO←→2Bi2O3+2Ni2O3+O2
と表すこともできる。
上記実施の形態では酸化ニッケルと酸化ビスマスの混合層をホール注入層として用いたが、本発明は、この組み合わせに限定されるものではない。例えば、Biのように最大価数とそれより少ない価数で安定する元素として、Pb、Tl、In、Sn、Sbが挙げられる。これらの元素は、最外殻のs軌道に電子対を形成した状態が最も安定することが知られている(不活性電子対効果)。このため、最大価数状態(最外殻のs軌道から電子を全て奪われた状態)とともに、さらに安定する2少ない価数状態(最外殻のs軌道に不活性電子対が形成された状態)を持ち、従って、本実施の形態のBiと同様の効果を得ることができるものと考えられる。
2.ホールオンリー素子
10,20.基板
11,21.陽極
12,22.ホール注入層
13.バンク
14,24.バッファ層
15,25.発光層
16,26.陰極
16a.バリウム層
16b.アルミニウム層
17,27.直流電源
Claims (6)
- 互いに間隔をあけて対向配置された陽極および陰極と、
有機材料を含んでなり、前記陽極と前記陰極との間に介挿された機能層と、
当該機能層にホールを注入する機能を有し、前記陽極と前記機能層との間に介挿されたホール注入層と、
を備え、
前記ホール注入層は、第1の酸化物と第2の酸化物とを含有する混合層であり、
前記第1の酸化物は、p型の金属酸化物であり、
前記第2の酸化物は、その組成中に含まれる元素が、最大価数を取る第1状態と、前記最大価数よりも少ない価数を取る第2状態の何れにおいても熱的に安定であり、且つ、前記第2状態が前記第1状態よりも熱的に安定であり、
前記ホール注入層に含有される前記第2の酸化物は、前記第1状態で前記元素を含む
ことを特徴とする有機EL素子。 - 前記第2の酸化物の組成中に含まれる前記元素においては、前記最大価数と、それよりも少ない価数の差が2である、
請求項1記載の有機EL素子。 - 前記第2の酸化物の組成中に含まれる前記元素は、最外殻のs軌道に電子対を形成した状態が最も安定する元素である、
請求項1記載の有機EL素子。 - 前記第2の酸化物の組成中に含まれる前記元素は、Tl、Pb、Bi、Se、In、Sn、Sbである、
請求項1記載の有機EL素子。 - 前記第1の酸化物の組成中には、Ni、Cu、Co、Fe、Cr、Mnの少なくとも一種の元素を含む、
請求項1記載の有機EL素子。 - 前記第1の酸化物の組成中に含まれる元素は、前記第2の酸化物の組成中に含まれる前記元素よりもイオン化傾向が高い、
請求項1記載の有機EL素子。
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US20140175411A1 (en) | 2014-06-26 |
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US9035293B2 (en) | 2015-05-19 |
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