WO2003101158A1 - Substrat comprenant un film conducteur transparent et dispositif electroluminescent organique - Google Patents

Substrat comprenant un film conducteur transparent et dispositif electroluminescent organique Download PDF

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Publication number
WO2003101158A1
WO2003101158A1 PCT/JP2003/006763 JP0306763W WO03101158A1 WO 2003101158 A1 WO2003101158 A1 WO 2003101158A1 JP 0306763 W JP0306763 W JP 0306763W WO 03101158 A1 WO03101158 A1 WO 03101158A1
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Prior art keywords
transparent conductive
substrate
conductive film
film
organic
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PCT/JP2003/006763
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English (en)
Japanese (ja)
Inventor
Kunio Masumo
Akira Mitsui
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Asahi Glass Company, Limited
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Application filed by Asahi Glass Company, Limited filed Critical Asahi Glass Company, Limited
Priority to JP2004507295A priority Critical patent/JPWO2003101158A1/ja
Priority to AU2003241911A priority patent/AU2003241911A1/en
Publication of WO2003101158A1 publication Critical patent/WO2003101158A1/fr

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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
    • H10K50/80—Constructional details
    • H10K50/805—Electrodes
    • H10K50/81—Anodes

Definitions

  • the present invention relates to a substrate with a transparent conductive film used as an electrode for an organic EL device and an organic EL device. Background technology
  • This organic EL device usually includes an anode, a light-emitting layer, and a cathode, and has a thin film laminate including a hole injection layer, a hole transport layer, an electron transport layer, an electron injection layer, and the like as necessary.
  • Means The organic EL device has a voltage of about 100 V
  • the anode is formed by forming a transparent conductive film on a transparent substrate such as glass.
  • the transparent conductive film include a transparent conductive film mainly containing an oxide of indium and tin (hereinafter referred to as an IT film), a transparent conductive film mainly containing an oxide of zinc and indium, and the like.
  • IT film transparent conductive film mainly containing an oxide of indium and tin
  • the ITO film is excellent in conductivity, high in visible light transmittance, and excellent in chemical resistance, but has an excellent feature that it is soluble in a certain kind of acid, so that it can be easily patterned.
  • the ITO film is preferably crystalline.
  • crystalline films tend to have irregularities on the surface.
  • large irregularities on the ITO film surface may cause problems such as leak current and dark spots.
  • an ITO film is formed at a relatively low temperature of 100 to 150, and then heat-treated at 100 to 450, and It has been proposed that the crystal orientation of the film be (111) orientation.
  • the organic EL device is a charge injection type device, it is desired that the electrical characteristics of the ITO film not only include the electric resistance but also the charge injection characteristics into the organic EL device. If the charge injection at the electrodes is good, the driving voltage is reduced, the power consumption is low, and a highly reliable organic EL device can be manufactured.
  • Japanese Patent Application Laid-Open No. 8-167479 discloses an invention relating to an ITO film in which the work function of an anode surface used in an organic EL device or the like is increased to 5.1 to 6.0 eV by plasma irradiation or the like. .
  • Japanese Patent Application Laid-Open No. 2000-26119 describes that it is appropriate that the carrier concentration in a conductive oxide thin film used as an anode is 1 ⁇ 10 18 cm ⁇ 3 to 1 ⁇ 10 22 cm ⁇ 3. ing.
  • the driving voltage of the organic EL element does not necessarily decrease, and the carrier concentration in the film is similarly reduced. It was found that the driving voltage of the organic EL element did not necessarily decrease even if the range was appropriate.
  • an object of the present invention is to provide an organic EL device using a substrate with an ITO film having a high luminance and a low driving voltage. Disclosure of the invention
  • the present invention relates to a substrate with a transparent conductive film formed by forming a transparent conductive film mainly containing an oxide of indium and tin on a substrate, wherein the transparent conductive film obtained by a Mott-Schottky method is provided. providing a transparent conductive film-coated substrate, wherein the surface carrier concentration of the film 1. is 0 X 1 0 21 ⁇ 1. 0 X 1 0 23 cm one 3.
  • the present invention provides an organic EL device in which an anode, a light-emitting layer, and a cathode are formed in this order, wherein the anode is the substrate with a transparent conductive film. Further, the present invention provides an organic EL device in which an anode, a hole injection layer, a hole transport layer, a light emitting layer, and a cathode are formed in this order, wherein the anode has the transparent conductive film.
  • the present invention provides an organic EL device, which is a substrate, wherein the hole injection layer is copper phthalocyanine.
  • a transparent conductive film mainly containing an oxide of indium and tin is formed on a substrate.
  • a method for producing a substrate with a transparent conductive film characterized in that a substrate with a transparent conductive film having a surface carrier concentration of 1. OX 10 21 to 1. OX 10 23 cm ⁇ 3 determined by a method is obtained. I will provide a. BRIEF DESCRIPTION OF THE FIGURES
  • FIG. 1 is a schematic cross-sectional view showing an example of a substrate with an ITO film according to the present invention.
  • the substrate 10 with an ITO film according to the present invention has an ITO film 50 formed on a substrate 20, and further has an alkali barrier layer in contact with the substrate 20 between the substrate 20 and the ITO film.
  • (Layer for preventing alkali ions in the substrate from diffusing into the ITO film) 30 may be formed, or between the substrate 20 and the ITO film 50, the base film 40 may be in contact with the ITO film 50. It may be formed.
  • the substrate of the ITO film in the present invention is not particularly limited, and examples thereof include an inorganic transparent substrate such as a glass substrate and an organic transparent substrate such as a plastic substrate.
  • the glass substrate include an alkali-containing glass substrate such as a soda lime silicate glass substrate, and a non-alkali glass substrate such as a borosilicate glass substrate.
  • the average surface roughness Ra is preferably about 0.1 to 5 nm.
  • the average surface roughness Ra is preferably about 0.1 to 10 nm.
  • the average surface roughness Ra is measured according to JISB 0601.
  • the cut-off value is 0.8 zm and the evaluation length is 2.4 / m.
  • an alkali-containing glass substrate When an alkali-containing glass substrate is used, contact the glass substrate on top of the glass substrate to prevent alkali ions contained in the glass substrate from diffusing into the ITO film and affecting the resistance of the ITO film. It is preferable to form a silicon oxide (SiO 2 ) film or the like as an alkali barrier layer.
  • SiO 2 silicon oxide
  • the method for forming the alkali barrier layer is not particularly limited, and examples thereof include a thermal decomposition method (a method of forming a film by applying a raw material solution and then heating), a CVD method, a sputtering method, a vapor deposition method, and an ion plating method.
  • a thermal decomposition method a method of forming a film by applying a raw material solution and then heating
  • a CVD method a method of forming a film by applying a raw material solution and then heating
  • a CVD method a method of forming a film by applying a raw material solution and then heating
  • a CVD method a chemical vapor deposition method
  • a sputtering method a vapor deposition method
  • an ion plating method for example, in the case of a SiO 2 film, a film forming method such as an RF (high frequency) sputtering method using a SiO 2 target or an RF or DC (direct current) s
  • the sputtering gas may prescribe gas ratio of A r- 0 2 mixed with a gas, S i 0 so 2 film becomes transparent film without absorption A r and O z preferable.
  • the thickness of the alkali barrier layer (hereinafter, the thickness means a geometric thickness) is preferably 10 nm or more from the viewpoint of alkali barrier performance, and preferably 500 nm or less from the viewpoint of cost.
  • the average surface roughness R a of the alkali-containing glass substrate alkali barrier layer is formed is preferably 0. 1 to 10 nm.
  • the ITO film is a film mainly containing an oxide of indium and tin.
  • a film containing 1 to 20% by mass of tin oxide with respect to the total amount of (indium oxide + tin oxide) is preferable. It is listed as.
  • the thickness of the ITO film is preferably from 100 to 500 nm, more preferably from 100 to 300 nm, and still more preferably from 150 to 220 nm, from the viewpoints of resistance value, transmittance and the like.
  • the specific resistance is preferably 4 ⁇ 10 ⁇ 4 ⁇ cm or less, and the sheet resistance is preferably 20 ⁇ or less.
  • the method for forming the ITO film is not particularly limited, and examples thereof include a thermal decomposition method, a CVD method, a sputtering method, an evaporation method, and an ion plating method.
  • a thermal decomposition method for example, a method in which an ITO target is used and a high frequency (RF) or direct current (DC) sputtering method is used.
  • RF radio frequency
  • DC direct current
  • the substrate temperature at the time of sputtering the ITO film is preferably 100 to 500 ° C., particularly preferably. If the substrate temperature is less than 100, the ITO film tends to be amorphous, and the chemical resistance of the ITO film is reduced. If the substrate temperature exceeds 500 ° C, the crystallinity will be promoted, and the unevenness of the ITO film surface will increase.
  • a base film may be provided between the substrate and the ITO film in contact with the ITO film.
  • the underlayer is preferably a film containing zirconium oxide as a main component.
  • the base film may contain impurities such as Hf, Fe, Cr, Y, Ca, and Si, and the total amount of the impurities is the total amount of Zr and the total amount of the impurities. On the other hand, it is preferably at most 10 atomic%, particularly preferably at most 1 atomic%.
  • the thickness of the underlayer is preferably from 1 to 150 nm. If the film thickness is less than 1 nm, the effect of improving the surface carrier concentration is not sufficient, and if it exceeds 150 nm, it is not preferable in terms of cost.
  • the thickness of the base film means an average film thickness, and the same applies to a case where the film is not a continuous film. By the base film of the film thickness is present, it is possible to control the average surface roughness R a of the surface of the resulting conductive film substrate with a 0. 1 ⁇ 3. 0 nm.
  • the thickness of the underlayer is more preferably 1 to 15 nm.
  • the underlayer film of the present invention affects the crystal growth of the ITO film formed thereon, can change the crystal orientation of the ITO film, and improves the flatness of the surface of the obtained substrate with a conductive film. Contribute.
  • the method for forming the underlayer is not particularly limited, and examples thereof include a thermal decomposition method, a CVD method, a sputtering method, a vapor deposition method, and an ion plating method.
  • Examples of the formation method include a method of forming by RF or DC sputtering using a metal Zr target and a method of forming by RF sputtering using a stabilized zirconia target. It is preferable to use the DC sputtering method from the viewpoint of the film speed.
  • the organic EL device includes an anode having a transparent conductive film formed on a substrate, a light emitting layer, and a cathode, and as necessary, a hole injection layer, a hole transport layer, an electron transport layer, and an electron injection layer. It means an element having a laminate of thin films including layers and the like.
  • Examples of the organic EL element include: 1) an element in which an anode, a light emitting layer, and a cathode are formed in this order; 2) an anode, a hole injection layer, a hole transport layer, a light emitting layer, and a cathode. 3) A device in which an anode, a hole injection layer, a hole transport layer, an electron injection layer, a light emitting layer, and a cathode are formed in this order.
  • an organic EL device having high luminance, low driving voltage, low power consumption, and high reliability can be obtained.
  • the present inventors newly show that the carrier voltage and work function in the film are not dominant, and that the drive voltage of the organic EL device can be reduced by improving the surface carrier concentration of the ITO film. I found it.
  • the surface carrier concentration can be obtained by calculation by measuring the capacity of a depletion layer generated on the film surface. For example, the electrode and the substrate and the silver wire with I TO membrane, the electrolyte solution (1 mol ⁇ liter ⁇ including L i C 10 4 - butyrolactone solution) in, I TO membrane surface upon application of a variety of voltage
  • the capacitance of the depletion layer generated in the above condition is measured with an impedance analyzer, and the surface carrier concentration N can be obtained from the following equation (1) of Mott-Shottky.
  • the method of determining the surface carrier concentration by the following equation (1) of the motto key is called the motto shot key method.
  • C is the capacitance of the depletion layer (F)
  • ⁇ is the flat band voltage (V)
  • V is the applied voltage (V)
  • ⁇ is the relative dielectric constant of the ITO film
  • ⁇ is the relative dielectric constant of the ITO film
  • ⁇ is the relative dielectric constant of the ITO film
  • ⁇ is the relative dielectric constant of the ITO film
  • Q is the elementary charge (1. 602 X 10- 19 C)
  • N denotes the surface carrier concentration (m_ 3).
  • the surface carrier concentration of I TO film obtained by the motto Schottky one method and 1. 0 X 10 21 ⁇ 1. 0 X 10 23 cm_ 3, the I TO film coated substrate as an organic EL element electrode (anode)
  • the driving voltage can be reduced without lowering the luminance of the organic EL element.
  • the surface carrier concentration is set to 1.0 ⁇ 10 21 to 1.0 ⁇ 10 22 cm ⁇
  • the surface carrier concentration of the ITO film of the present invention is influenced by the manufacturing conditions of the ITO film, such as the substrate temperature and impurities contained in the film, but which conditions are dominant. It is not clearly known if any. It has also been clarified that the surface carrier concentration can be improved by providing a base film containing zirconium oxide as the main component in contact with the ITO film, but the reason for this is clearly understood. Absent.
  • the material of the hole transport layer is not particularly limited as long as it has a hole injection or electron barrier property.
  • a hole injection layer between the anode and the hole transport layer for the purpose of reducing the hole injection barrier and improving the adhesion.
  • the material for the hole injection layer include phthalocyanines such as copper phthalocyanine, 4, 4 ', 4,, tris (N- (3-methylphenyl) -N-phenylamino) triphenylamine, 4, 4, and , 4 ', -Tris (N, N-diphenylamino) Starburst amines such as triphenylamine can be used.
  • phthalocyanines such as copper phthalocyanine, 4, 4 ', 4,, tris (N- (3-methylphenyl) -N-phenylamino) triphenylamine, 4, 4, and , 4 ', -Tris (N, N-diphenylamino) Starburst amines such as triphenylamine can be used.
  • copper phthalocyanine as the material of the hole injection layer in view of the reliability of the device and the
  • the material of the light emitting layer is not particularly limited as long as it is a material having a light emitting ability, and examples thereof include tris (8-quinolinol) aluminum (A 1 Q 3).
  • a 1 Q 3 is used as the light emitting layer, the light emitting layer also functions as an electron transport layer Good.
  • the light emitting layer may be doped with various dyes for the purpose of improving the luminous efficiency and the device life.
  • L i F The material for the electron injection layer, L i F, such as L i 2 0, Na 2 0 is illustrated, is formed by vapor deposition method or the like.
  • a metal or an alloy having a small work function is preferably used, and A1Li, MgAg and the like are exemplified, and a film is formed by a vapor deposition method or the like.
  • a washed soda lime silicate glass substrate (average surface roughness Ra : 0.5 nm) was set in a sputtering apparatus, the substrate was heated to 220, and the substrate temperature during sputtering was maintained at 220.
  • a SiO 2 film was formed as an alkali barrier layer by an RF sputtering method using a SiO 2 target.
  • the spa Tsu evening ring gas was used A r- 0 2 mixed gas.
  • Ar and 0 2 gas ratio, Ar: 0 2 70: 30 and (volume ratio) was the total pressure and 0. 67 P a. 2.
  • Discharge was performed at 8 WZcm 2 to form a film.
  • the film thickness was 20 nm.
  • the average surface roughness R a of the S i 0 2 of the film-coated substrate S i 0 2 film surface was 0. 5 nm.
  • the Z R_ ⁇ 2 film was formed by RF sputtering as a base film.
  • a metal Zr target was used as the target.
  • an ITO film was formed by a sputtering method in contact with the base film.
  • the target was an ITO target.
  • Composition of I TO targets used were those Sn_ ⁇ 2 is 10% by mass of the total amount of (I n 2 0 3 + S N_ ⁇ 2).
  • the spa Tsu evening ring gas was used Ar- 0 2 mixed gas.
  • Discharge was performed at 4 WZcm 2 to form a film.
  • the composition of the formed ITO film was equivalent to the composition of the evening gate.
  • the film thickness was 18 O nm.
  • a substrate having an ITO film was formed by performing the same treatment as in Example 1 except that the oxygen plasma treatment was not performed.
  • Example 2 Except for not forming the Z r0 2 film as a base film, was treated in the same manner as Example 1 to form a substrate-out with I TO film.
  • a substrate with an ITO film was formed in the same manner as in Example 1, except that an argon plasma treatment was performed using a simple plasma apparatus before the oxygen plasma treatment. Compared with Example 1, the surface carrier concentration of the ITO film was reduced by the argon plasma treatment.
  • a substrate with an ITO film was formed in the same manner as in Example 3, except that an argon plasma treatment was performed using a simple plasma apparatus before the oxygen plasma treatment. Compared with Example 3, the argon plasma treatment reduced the surface carrier concentration of the ITO film.
  • the obtained substrate with an ITO film was evaluated by the following method.
  • the thickness d of the depletion layer of the ITO film can be obtained by equation (2).
  • d is the thickness of the depletion layer (m)
  • ⁇ is the relative permittivity of the ITO film
  • ⁇ is the relative permittivity of the ITO film
  • ⁇ is the relative permittivity of the ITO film
  • ⁇ is the relative permittivity of the ITO film
  • ⁇ is the relative permittivity of the ITO film
  • ⁇ is the relative permittivity of the ITO film
  • ⁇ is the relative permittivity of the ITO film
  • ⁇ The induced lightning constant of vacuum (8. 854 X 10- 12 C / Vm)
  • S is a measurement area (m 2)
  • C is the depletion layer Indicates the capacity (about 5 F).
  • the thickness d of the depletion layer is calculated to be about 1 nm from the above equation (2). From these results, it was found that the surface carrier concentration of the ITO films of Examples 1 to 5 was as small as about 1 nm.
  • Sheet resistance value measured by a four-point needle method.
  • Table 1 shows the characteristic evaluation results of the obtained ITO film.
  • the ITO film of the substrate (anode) with the IT ⁇ film formed in Examples 1 to 5 was patterned to create a light-emitting part (2 mm square) and a wiring part.
  • Patterning A mask for patterning was set on the patterned ITO film so that it overlapped the light emitting portion of the ITO film but did not overlap the wiring portion.
  • copper phthalocyanine was sequentially deposited to a thickness of 10 nm as a hole injection layer, and 4,4'-bis (N- (1-naphthyl) -1-N-phenylamino) biphenyl (Hiichi NPD) was deposited as a hole transport layer.
  • the ITO film of the substrate (anode) with the ITO film formed in Examples 1 and 4 was patterned to create a light-emitting part (2 mm square) and a wiring part.
  • a mask for patterning was set on the patterned ITO film so that it overlapped the light emitting part of the ITO film but did not overlap the wiring part.
  • copper phthalocyanine is sequentially used as a hole injection layer with a thickness of 10 nm as a hole injection layer, and N, N, 1-di (phenanthrene-1-yl) -1N, N, 1-diphenyl-1, 1'- is used as a hole transport layer.
  • Biphenyl-4,4'-diamine is 80 nm thick
  • tris (8-quinolinol) aluminum is 60 nm thick as an emission layer and an electron transport layer
  • LiF is used as an electron injection layer.
  • Organic EL device B was obtained by depositing A1 as a cathode with a thickness of 5 nm and a thickness of 80 nm.
  • the obtained organic EL device was evaluated by the following method.
  • Table 2 shows the characteristic evaluation results of the obtained organic EL element A
  • Table 3 shows the characteristic evaluation results of the organic EL element B.
  • the organic EL devices using the substrate with the ITO film (ITO film with high surface carrier concentration) of Examples 1 to 3 as the anode are the ITO films of Examples 4 and 5 (ITO film with low surface carrier concentration).
  • the driving voltage is lower than that of the organic EL device using the attached substrate as an anode, while maintaining the same brightness. A similar tendency is seen in the results of Examples 1 and 4 in Table 3.
  • an organic EL device having high luminance, low driving voltage, low power consumption, and high reliability can be manufactured.
  • an electrode having a low surface roughness an organic EL device having high luminance, low driving voltage, low power consumption, and high reliability can be manufactured.

Abstract

L'invention concerne un dispositif électroluminescent organique qui comporte un substrat comprenant un film ITO, ce dispositif possédant une luminance élevée, avec une faible tension de commande, présentant une faible consommation d'énergie et une haute fiabilité. L'invention concerne également un substrat sur lequel est formé un film conducteur transparent contenant majoritairement un oxyde d'indium et d'étain, la concentration des supports de surface de ce film conducteur transparent déterminée par la méthode de Mott-Schottky étant comprise entre 1,0 1021 et 1,0 1023 cm-3. L'invention concerne en outre un dispositif électroluminescent organique formé d'une anode constituée par un substrat comprenant le film conducteur transparent, d'une couche luminescente et d'une cathode, disposées dans cet ordre.
PCT/JP2003/006763 2002-05-29 2003-05-29 Substrat comprenant un film conducteur transparent et dispositif electroluminescent organique WO2003101158A1 (fr)

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JP2004507295A JPWO2003101158A1 (ja) 2002-05-29 2003-05-29 透明導電膜付き基板および有機ｅｌ素子
AU2003241911A AU2003241911A1 (en) 2002-05-29 2003-05-29 Substrate with transparent conductive film and organic el device

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JP2002155793 2002-05-29

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JP2005276446A (ja) * 2004-03-22 2005-10-06 Fuji Electric Holdings Co Ltd 有機ｅｌディスプレイおよびその製造方法
JP2007287450A (ja) * 2006-04-14 2007-11-01 Nippon Soda Co Ltd 透明導電性基材
JP2009224595A (ja) * 2008-03-17 2009-10-01 Fujifilm Corp 有機電界発光表示装置及びその製造方法
JP2010050279A (ja) * 2008-08-21 2010-03-04 Denso Corp 有機ｅｌ素子及び有機ｅｌ素子の製造方法
JP2011077043A (ja) * 2004-03-23 2011-04-14 Toyota Central R&D Labs Inc 電極
JP7470677B2 (ja) 2018-09-24 2024-04-18 ファースト・ソーラー・インコーポレーテッド テクスチャ化ｔｃｏ層を有する光起電デバイス、およびｔｃｏスタックを作る方法

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JP7470677B2 (ja) 2018-09-24 2024-04-18 ファースト・ソーラー・インコーポレーテッド テクスチャ化ｔｃｏ層を有する光起電デバイス、およびｔｃｏスタックを作る方法

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JPWO2003101158A1 (ja) 2005-09-29
AU2003241911A1 (en) 2003-12-12

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