WO2017094547A1 - Procédé de fabrication d'élément de conversion photoélectrique - Google Patents

Procédé de fabrication d'élément de conversion photoélectrique Download PDF

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WO2017094547A1
WO2017094547A1 PCT/JP2016/084475 JP2016084475W WO2017094547A1 WO 2017094547 A1 WO2017094547 A1 WO 2017094547A1 JP 2016084475 W JP2016084475 W JP 2016084475W WO 2017094547 A1 WO2017094547 A1 WO 2017094547A1
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layer
thin film
photoelectric conversion
electrode
organic
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PCT/JP2016/084475
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English (en)
Japanese (ja)
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細野　秀雄
日出也 雲見
中村　伸宏
暁 渡邉
俊成 渡邉
宮川　直通
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国立大学法人東京工業大学
旭硝子株式会社
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Application filed by 国立大学法人東京工業大学, 旭硝子株式会社 filed Critical 国立大学法人東京工業大学
Priority to CN201680069408.1A priority Critical patent/CN108293281B/zh
Priority to JP2017553783A priority patent/JP6729602B2/ja
Priority to KR1020187014679A priority patent/KR20180087259A/ko
Publication of WO2017094547A1 publication Critical patent/WO2017094547A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • 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
    • 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
    • H05B33/26—Light sources with substantially two-dimensional radiating surfaces characterised by the composition or arrangement of the conductive material used as an electrode
    • 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]

Definitions

  • the present invention relates to a method for manufacturing a photoelectric conversion element, and particularly relates to a method for manufacturing a photoelectric conversion element such as an electroluminescence element and a solar cell.
  • Photoelectric conversion elements are widely used in various fields such as electroluminescence elements that emit light when voltage is applied and solar cells that generate electromotive force when light is incident thereon.
  • a light emitting diode which is a kind of electroluminescence element, includes a pair of electrodes (anode and cathode) and a light emitting layer disposed between these electrodes.
  • a voltage is applied between both electrodes, holes and electrons are injected from each electrode into the light emitting layer.
  • the holes and electrons recombine in the light emitting layer, binding energy is generated, and the light emitting material in the light emitting layer is excited by this binding energy. Light emission occurs when the excited luminescent material returns to the ground state. Therefore, the LED can be used as a light emitting element or illumination.
  • the solar cell has a pair of electrodes and a photoelectric conversion layer disposed between them.
  • the photoelectric conversion layer When light enters the photoelectric conversion layer, holes and electrons are generated in the photoelectric conversion layer, and an electromotive force is generated. Electric power can be taken out of the system by taking out holes and electrons from separate electrodes.
  • Patent Document 1 In the field of photoelectric conversion elements such as LEDs and solar cells, various configurations have been proposed in order to further improve the characteristics as elements (for example, Patent Document 1).
  • Patent Document 1 describes that, in a photoelectric conversion element, an oxide amorphous thin film containing zinc (Zn) and silicon (Si) is used for an electron transport layer or the like.
  • the present invention has been made in view of such a background, and an object of the present invention is to provide a method for manufacturing a photoelectric conversion element having significantly improved characteristics as compared with the prior art.
  • a method for producing a photoelectric conversion element (1) disposing a first electrode on a substrate; (2) The upper portion of the first electrode is made of a metal oxide containing zinc (Zn) and oxygen (O), and further containing at least one of silicon (Si) and tin (Sn). Disposing a first thin film; (3) applying pressure by gas to the substrate having the first electrode and the first thin film; (4) Arranging a photoelectric conversion layer that is a layer that converts an applied voltage into light or a layer that converts incident light into electric power on the first thin film; (5) disposing a second electrode on the photoelectric conversion layer; Is provided.
  • a method for producing a photoelectric conversion element comprising: (1) disposing a first electrode on a substrate; (2) The upper portion of the first electrode is made of a metal oxide containing zinc (Zn) and oxygen (O), and further containing at least one of silicon (Si) and tin (Sn). Disposing a first thin film; (3) applying pressure by gas to the substrate having the first electrode and the first thin film; (4) Arranging a photoelectric conversion layer that is a layer that converts an applied voltage into light or a layer that converts incident light into electric power on the first thin film; (5) disposing a second electrode on the photoelectric conversion layer; Is provided.
  • the “photoelectric conversion element” means a generic name of elements having a “photoelectric conversion layer”.
  • the “photoelectric conversion layer” is a layer that generates electric energy when electric energy is introduced (applied), as well as a layer that generates electric energy when light energy is introduced (irradiated). (Electro-optical conversion layer) is also included.
  • the “photoelectric conversion layer” is composed of a light-emitting layer that emits light when a voltage is applied
  • the “photoelectric conversion element” including the “photoelectric conversion layer” is an electroluminescence element (EL element).
  • EL element may be an organic EL element in which the “photoelectric conversion layer” is composed of an organic light emitting layer, or an inorganic EL element in which the “photoelectric conversion layer” is composed of an inorganic light emitting layer. Good.
  • the “photoelectric conversion element” including such a “photoelectric conversion layer” is a solar cell.
  • a solar cell may be an organic solar cell in which the “photoelectric conversion layer” is composed of an organic layer or an inorganic solar cell in which the “photoelectric conversion layer” is composed of an inorganic layer.
  • the characteristics as an element can be significantly improved as compared with the prior art.
  • the manufacturing method according to an embodiment of the present invention will be described in detail by taking as an example the case where the photoelectric conversion element is an electroluminescence element and a solar cell.
  • first manufacturing method Metal for Manufacturing EL Element According to One Embodiment of the Present Invention
  • FIG. 1 schematically shows an example of the flow of the first manufacturing method.
  • FIG. 2 schematically shows a cross section of an EL element manufactured by the first manufacturing method.
  • the first manufacturing method is: (A) disposing the first electrode on the substrate (step S110); (B)
  • the first electrode is made of a metal oxide containing zinc (Zn) and oxygen (O), and further comprising at least one of silicon (Si) and tin (Sn).
  • step S120 Placing the thin film 1 (step S120); (C) applying a pressure by gas to the substrate having the first electrode and the first thin film (step S130); (D) disposing a first additional layer on top of the first thin film (step S140); (E) disposing an organic light emitting layer on top of the first additional layer (step S150); (F) placing a second additional layer on top of the organic light emitting layer (step S160); (G) disposing a second electrode on top of the second additional layer (step S170); In this order.
  • a first electrode (cathode) 120 for example, on a substrate 110, a first electrode (cathode) 120, a first thin film 130, a first additional layer 140, an organic light emitting layer 150, a first The organic EL element 100 including the two additional layers 160 and the second electrode (anode) 170 in this order is manufactured.
  • Step S110 First, the substrate 110 is prepared.
  • the substrate 110 has a role of supporting each layer constituting the organic EL element 100 on the upper part.
  • the material of the substrate 110 is not particularly limited.
  • the substrate 110 is made of a transparent material.
  • a glass substrate or a plastic substrate is used as the substrate 110.
  • the first electrode 120 is disposed on the substrate 110.
  • the first electrode 120 is usually made of metal.
  • the first electrode 120 is made of a transparent material.
  • a transparent metal oxide thin film such as ITO (indium tin oxide) is used.
  • the first electrode 120 is, for example, aluminum, silver, gold, magnesium, calcium, titanium, yttrium, lithium, gadolinium, ytterbium, ruthenium, manganese, molybdenum, vanadium, chromium, tantalum, or an alloy of the aforementioned metals. Any metal material may be used.
  • the first electrode 120 may be, for example, ITO, antimony oxide (Sb 2 O 3 ), zirconium oxide (ZrO 2 ), tin oxide (SnO 2 ), zinc oxide (ZnO), or IZO (Indium Zinc).
  • Oxide Oxide
  • AZO ZnO—Al 2 O 3 : zinc oxide doped with aluminum
  • GZO ZnO—Ga 2 O 3 : zinc oxide doped with gallium
  • Nb-doped TiO 2 Nb-doped TiO 2
  • metal oxides such as IWZO (In 2 O 3 —WO 3 —ZnO: indium oxide doped with tungsten trioxide and zinc oxide).
  • the installation method of the first electrode 120 is not particularly limited.
  • the first electrode 120 may be formed by, for example, a vapor deposition method (vacuum vapor deposition method and electron beam vapor deposition method), an ion plating method, a laser ablation method, a sputtering method, or the like.
  • a vapor deposition method vacuum vapor deposition method and electron beam vapor deposition method
  • an ion plating method a laser ablation method
  • a sputtering method or the like.
  • the thickness of the first electrode 120 is in the range of 50 nm to 150 nm. If it is 50 nm or more, a low-resistance electrode is formed, which is preferable. If it is 150 nm or less, the step of the edge of the electrode is small, the coverage of a film to be formed later is good, and the light emitting area or light receiving area can be widened, which is preferable.
  • the thickness of the first electrode 120 is preferably in the range of 2 nm to 50 nm. If it is 2 nm or more, since the electroconductivity applicable as a photoelectric conversion element is obtained, it is preferable. If it is 50 nm or less, since transparency can be ensured, it is preferable.
  • Step S120 Next, the first thin film 130 is disposed on the first electrode 120.
  • the first thin film 130 is made of a metal oxide containing zinc (Zn) and oxygen (O), and further containing at least one of silicon (Si) and tin (Sn).
  • the first thin film 130 is formed using a metal oxide containing zinc (Zn), silicon (Si), and oxygen (O) (hereinafter referred to as ZSO), an oxide semiconductor such as ZnO that is generally used.
  • the work function is as low as, for example, 3.5 eV, and particularly excellent in the electron injection characteristics into the organic material.
  • the value of Zn / (Zn + Si) is, for example, in the range of 0.30 to 0.95 in terms of molar ratio. If it is 0.30 or more, a sufficiently large electron mobility can be obtained, and an increase in driving voltage of the photoelectric conversion element can be suppressed. If it is 0.95 or less, since a smooth surface is obtained, a short circuit can be suppressed.
  • the value of Zn / (Zn + Si) may be 0.70 to 0.94, 0.80 to 0.92, or 0.85 to 0.90 in molar ratio. .
  • x 0.30 or more, a sufficiently large electron mobility can be obtained, and an increase in driving voltage of the photoelectric conversion element can be suppressed.
  • x 0.95 or less, a particularly smooth surface can be obtained, so that a short circuit can be suppressed.
  • x may be 0.70 to 0.94, 0.80 to 0.92, or 0.85 to 0.90.
  • the first thin film 130 is preferably in the form of a complex oxide.
  • the first thin film 130 is composed of a metal oxide containing zinc (Zn), tin (Sn), and oxygen (O) (hereinafter referred to as ZTO), the etching rate is appropriate, and the first thin film 130 is not etched excessively. Since a desired shape can be formed, an organic EL element or a solar cell can be stably produced.
  • the first thin film 130 preferably has an SnO 2 content of 15 mol% or more and 95 mol% or less with respect to a total of 100 mol% of ZnO and SnO 2 in terms of oxide. If SnO 2 is 15 mol% or more, the crystallization temperature is high, and it is difficult to crystallize in the heat treatment step performed in various processes.
  • SnO 2 is less 95 mol%, in easy sintering, good oxide target is obtained, easy to form a thin film.
  • SnO 2 may be 30 mol% or more and 70 mol% or less, 35 mol% or more and 60 mol% or less, or 40 mol% or more and 50 mol% or less.
  • the work function is low, and Since the etching rate is appropriate and high transparency is obtained, the device characteristics of the organic EL device or solar cell are improved.
  • SnO 2 is 12 mol% or more and 97 mol% or less with respect to the total 100 mol% of ZnO, SnO 2 , and SiO 2 in terms of oxide. If SnO 2 is 15 mol% or more, the crystallization temperature is high, and it is difficult to crystallize in the heat treatment step performed in various processes.
  • SnO 2 is less 95 mol%, in easy sintering, good oxide target is obtained, easy to form a thin film.
  • SnO 2 may be 30 mol% or more and 70 mol% or less, 35 mol% or more and 60 mol% or less, or 40 mol% or more and 50 mol% or less.
  • the SiO 2 content is preferably 5 mol% or more and 30 mol% or less with respect to a total of 100 mol% of ZnO, SnO 2 and SiO 2 in terms of oxide. .
  • SiO 2 is 5 mol% or more, not more than 30 mol%, the electron affinity is not too high, the volume resistivity is not too high.
  • SiO 2 may be 7 mol% or more and 20 mol% or less, or 10 mol% or more and 15 mol% or less.
  • the first thin film 130 may further include one or more metal components selected from the group consisting of titanium (Ti), indium (In), gallium (Ga), niobium (Nb), and aluminum (Al). .
  • the content of these metal components calculated as oxide, ZnO, the total 100 mol% of SiO 2, SnO 2, and other oxides of the metal components, preferably not more than 15 mol%, more preferably 10mol % Or less, more preferably 5 mol% or less. In terms of oxides, these metals are calculated as TiO 2 , In 2 O 3 , Ga 2 O 3 , Nb 2 O 5 , or Al 2 O 3 .
  • the composition of the thin film of the first thin film 130 can be analyzed by performing substrate correction using EPMA when the film thickness is 200 nm or more.
  • the composition of the first thin film 130 can be analyzed using SEM-EDX at an acceleration voltage of 10 kV. Analysis can also be performed by performing substrate correction using XRF. Further, when using ICP, the first thin film 130 can be analyzed by using a volume of 1 mm 3 or more.
  • the first thin film 130 is dominant in an amorphous state or an amorphous state.
  • amorphous means a substance that does not give a sharp peak in X-ray diffraction measurement.
  • the X-ray wavelength ⁇ is 0.154 nm and the Scherrer constant K is 0.9
  • the crystallite diameter (Scherrer diameter) obtained by the Scherrer formula represented by the following formula (1) is 5. 2 nm or less.
  • the Scherrer diameter L is a Scherrer constant K, an X-ray wavelength ⁇ , a half-value width ⁇ , and a peak position ⁇ .
  • the amorphous state is dominant when the amorphous is present in a volume ratio of more than 50%. If the first thin film 130 is predominantly amorphous or amorphous, it is preferable because the film surface has high smoothness and can prevent a short circuit of the element.
  • the first thin film 130 may be a microcrystal or a form in which amorphous and microcrystal are mixed.
  • the microcrystal is a crystal having a Scherrer diameter larger than 5.2 nm and smaller than 100 nm.
  • the first thin film 130 be microcrystalline because conductivity is improved. It is preferable that the first thin film 130 be in a form in which amorphous and microcrystals are mixed because both smoothness and conductivity are improved.
  • the electron mobility of the first thin film 130 may be 10 ⁇ 4 cm 2 ⁇ V ⁇ 1 s ⁇ 1 to 10 2 cm 2 ⁇ V ⁇ 1 s ⁇ 1 and may be 10 ⁇ 3 cm 2 ⁇ V ⁇ 1. s -1 to 10 2 cm 2 ⁇ V -1 s -1 or 10 -2 cm 2 ⁇ V -1 s -1 to 10 2 cm 2 ⁇ V -1 s -1 .
  • the electron density of the first thin film 130 may be 1 ⁇ 10 18 cm ⁇ 3 to 1 ⁇ 10 21 cm ⁇ 3 , or 5 ⁇ 10 18 cm ⁇ 3 to 5 ⁇ 10 20 cm ⁇ 3. It may be 1 ⁇ 10 19 cm ⁇ 3 to 1 ⁇ 10 20 cm ⁇ 3 .
  • the first thin film 130 having such electron mobility and electron density is characterized by high conductivity and high electron transport properties.
  • the electron mobility of the first thin film 130 can be obtained by a hole measurement method, a time-of-flight (Time-of-Flight (TOF)) method, or the like.
  • the electron density of the first thin film 130 can be obtained by an iodine titration method or a Hall measurement method.
  • the electron affinity of the first thin film 130 may be 2.0 eV to 4.0 eV, 2.2 eV to 3.5 eV, or 2.5 eV to 3.0 eV.
  • the electron affinity is 2.0 eV or more, the electron injection characteristics of the first thin film 130 are improved, and the light emission efficiency of the organic EL element 100 is improved. Further, when the electron affinity is 4.0 eV or less, it is easy to obtain sufficient light emission from the organic EL element 100. From such a feature, by providing the first thin film 130, it is possible to improve the electron injection property with respect to the first electrode 120 in the organic EL element 100.
  • the ionization potential of the first thin film 130 may be 5.5 eV to 8.5 eV, 5.7 eV to 7.5 eV, or 5.9 eV to 7.0 eV.
  • the first thin film 130 having such a large ionization potential has a high hole blocking effect and can selectively transport only electrons. Therefore, the hole blocking property with respect to the first electrode 120 can be improved by installing the first thin film 130.
  • the thickness of the first thin film 130 is not limited to this, but may be 10 ⁇ m or less, 2 ⁇ m or less, 1 nm or more, or 10 nm or more. .
  • the first thin film 130 can be formed on the substrate 110 by, for example, a vapor deposition method using a target including zinc (Zn) and silicon (Si).
  • vapor deposition refers to vapor deposition of a target material including a physical vapor deposition (PVD) method, a PLD method, a sputtering method, and a vacuum deposition method, and then depositing this material on a substrate.
  • PVD physical vapor deposition
  • PLD physical vapor deposition
  • sputtering method a sputtering method
  • vacuum deposition method a vacuum deposition method
  • Sputtering methods include DC (direct current) sputtering method, high frequency sputtering method, helicon wave sputtering method, ion beam sputtering method, magnetron sputtering method and the like.
  • DC direct current
  • a thin film can be formed relatively uniformly in a large area.
  • the target only needs to contain Zn and Si.
  • Zn and Si may be contained in a single target or may be separately contained in a plurality of targets.
  • Zn and Si may exist as a metal or a metal oxide, respectively, or may exist as an alloy or a composite metal oxide.
  • the metal oxide or composite metal oxide may be crystalline or amorphous.
  • the target may contain one or more metal components selected from the group consisting of Sn, Ti, In, Ga, Nb, and Al in addition to Zn and Si.
  • Zn, Si and other metal components may be contained in a single target, or may be separately contained in a plurality of targets.
  • Zn, Si and other metal components may exist as a metal or a metal oxide, respectively, or may exist as an alloy or a composite metal oxide of two or more metals.
  • the metal oxide or composite metal oxide may be crystalline or amorphous.
  • the Zn / (Zn + Si) value in the target may be 0.30 to 0.95, 0.70 to 0.94, 0.80 in terms of molar ratio. It may be ⁇ 0.92 and may be 0.85 ⁇ 0.90.
  • a single target contains one or more metal components selected from the group consisting of Sn, Ti, In, Ga, Nb, and Al in addition to Zn and Si, the content of these metal components is oxide in terms of, ZnO, the total 100 mol% of an oxide of SiO 2 and other metal components, preferably not more than 15 mol%, more preferably not more than 10 mol%, more preferably not more than 5 mol%.
  • the metal component is calculated as SnO 2 , TiO 2 , In 2 O 3 , Ga 2 O 3 , Nb 2 O 5 , or Al 2 O 3 .
  • the composition analysis of the target can be performed by the XRF method or the like. Note that the composition of the formed first thin film 130 may differ from the composition ratio of the target used.
  • the first thin film 130 can be obtained by simultaneously sputtering a metal Si target and a ZnO target.
  • Other combinations of a plurality of targets include a combination of a ZnO target and a SiO 2 target, a combination of a plurality of targets including ZnO and SiO 2 with different ZnO ratios, a combination of a metal Zn target and a metal Si target, Examples include a combination of a metal Zn target and a SiO 2 target, and a combination of a metal Zn or metal Si target and a ZnO and SiO 2 target.
  • the first thin film 130 having a desired composition can be obtained by adjusting the power applied to each target.
  • the substrate 110 is not “positively” heated if the first thin film 130 is predominantly amorphous or amorphous. . This is because when the temperature of the substrate 110 rises, the first thin film 130 may not easily become amorphous.
  • the substrate 110 may be “incidentally” heated by the sputtering process itself such as ion bombardment. In this case, how much the temperature of the substrate 110 increases depends on the sputtering conditions. In order to avoid an increase in temperature of the substrate 110, the substrate 110 may be “positively” cooled. It is preferable that the first thin film 130 be formed at a substrate 110 temperature of 70 ° C. or lower. The temperature of the substrate 110 may be 60 ° C. or less, or 50 ° C. or less.
  • the pressure of the sputtering gas (pressure in the chamber of the sputtering apparatus) is preferably in the range of 0.05 Pa to 10 Pa, more preferably 0.1 Pa to 5 Pa, and further preferably 0.2 Pa to 3 Pa. If it is this range, since the pressure of sputtering gas will not be too low, plasma will become stable. Further, since the pressure of the sputtering gas is not too high, an increase in the temperature of the substrate 110 due to an increase in ion bombardment can be suppressed.
  • the sputtering gas used is not particularly limited.
  • the sputtering gas may be an inert gas or a noble gas. Oxygen may be contained.
  • the inert gas eg, N 2 gas.
  • examples of the rare gas include He (helium), Ne (neon), Ar (argon), Kr (krypton), and Xe (xenon). These may be used alone or in combination with other gases.
  • the sputtering gas may be a reducing gas such as NO (nitrogen monoxide) or CO (carbon monoxide).
  • the first thin film 130 can be formed on the first electrode 120.
  • Step S130 Next, a gas pressure is applied to the first thin film 130.
  • the value of the pressure applied to the first thin film 130 is, for example, in the range of 10 kPa to 1000 kPa, and may be, for example, atmospheric pressure (about 101 kPa). If the pressure applied to the 1st thin film 130 is 10 kPa or more, the light emission characteristic of organic EL will be improved and the power generation efficiency of a solar cell will improve. 50 kPa or more is preferable, and 80 kPa or more is more preferable. If the pressure applied to the 1st thin film 130 is 1000 kPa or less, the light emission characteristic of organic EL and the power generation efficiency of a solar cell can be improved, without using a large-scale high pressure application apparatus. 500 kPa or less is preferable, and 200 kPa or less is more preferable.
  • the gas may be air, nitrogen, oxygen, or the like.
  • the method for applying a gas pressure to the first thin film 130 is not particularly limited.
  • the pressure may be applied to the first thin film 130 by opening the chamber and removing the substrate 110 from the chamber.
  • the extracted substrate 110 may be exposed to, for example, room temperature air, nitrogen atmosphere, or oxygen atmosphere.
  • the temperature of the substrate may be raised when pressure is applied. Specifically, it is preferably 50 ° C to 300 ° C, more preferably 100 ° C to 200 ° C, and further preferably 120 ° C to 180 ° C.
  • Step S140 Next, the first additional layer 140 is disposed on the first thin film 130.
  • the first additional layer 140 may have at least one function of an electron injection layer, an electron transport layer, and a hole block layer.
  • step S140 is not an essential process, and may be omitted if unnecessary. That is, the 1st additional layer 140 is a layer which can be installed arbitrarily. This is because the first thin film 130 formed in step S120 described above can also function as an electron injection layer, an electron transport layer, and / or a hole block layer.
  • the organic EL element 100 having better characteristics can be provided by disposing the first additional layer 140. It becomes possible.
  • the first additional layer 140 When disposing the first additional layer 140 as an electron transport layer, the first additional layer 140 is selected from materials having electron transport properties.
  • a method for forming the electron transport layer a conventional general film forming method can be used.
  • the first additional layer 140 is selected from materials having an electron injection property.
  • the first additional layer 140 is, for example, one or more selected from the group consisting of lithium fluoride, cesium carbonate, sodium chloride, cesium fluoride, lithium oxide, barium oxide, barium carbonate, and 8-quinolinolato lithium. May be.
  • a method for forming the electron injection layer a conventional general film formation method can be used.
  • the first additional layer 140 is selected from materials having hole blocking properties.
  • the first additional layer 140 may be made of a material having a high HOMO level, for example.
  • the first additional layer 140 may be an inorganic oxide, a metal oxide, or the like.
  • Examples of the first additional layer 140 include IGZO (In—Ga—Zn—O), ITO (In—Sn—O), ISZO (In—Si—Zn—O), and IGO (In—Ga—O).
  • ITZO In—Sn—Zn—O
  • IZO In—Zn—O
  • IHZO In—Hf—Zn—O
  • As a method for forming the hole blocking layer a conventional general film forming method can be used.
  • the first additional layer 140 is preferably composed of an amorphous oxide electride containing calcium atoms and aluminum atoms.
  • Electron of amorphous oxide containing calcium atom and aluminum atom means an amorphous material composed of a solvate containing an electron composed of a calcium atom, an aluminum atom and an oxygen atom as a solvent and an electron as a solute. Means solid material. Electrons in the amorphous oxide act as anions. The electrons may exist as bipolarons. The bipolaron is configured by two cages adjacent to each other and electrons (solutes) included in each cage. However, the state of the amorphous oxide electride is not limited to the above, and two electrons (solutes) may be included in one cage.
  • a plurality of these cages may be aggregated, and the aggregated cage can be regarded as a microcrystal. Therefore, a state in which the microcrystal is included in the amorphous is also regarded as amorphous in the present invention.
  • the molar ratio (Ca / Al) of aluminum atoms to calcium atoms in the “amorphous oxide electride” thin film is preferably in the range of 0.3 to 5.0, and in the range of 0.55 to 1.00. More preferably, the range of 0.8 to 0.9 is more preferable, and the range of 0.84 to 0.86 is particularly preferable.
  • composition of “amorphous oxide electride” is preferably 12CaO ⁇ 7Al 2 O 3 , but is not limited thereto, and examples thereof include the following compounds (1) to (4).
  • metal atoms such as Sr, Mg, and / or Ba.
  • a compound in which some or all of Ca atoms are substituted with Sr is strontium aluminate Sr 12 Al 14 O 33 , and calcium strontium aluminum is used as a mixed crystal in which the mixing ratio of Ca and Sr is arbitrarily changed.
  • Nate Ca 12-x Sr X Al 14 O 33 (x is an integer of 1 to 11; in the case of an average value, it is a number greater than 0 and less than 12).
  • a part of metal atoms and / or nonmetal atoms (excluding oxygen atoms) in 12CaO.7Al 2 O 3 is Ti, V, One or more transition metal atoms selected from the group consisting of Cr, Mn, Fe, Co, Ni, and Cu or one or more alkali metal atoms selected from the group consisting of typical metal atoms, Li, Na, and K; Or an isomorphous compound substituted with one or more rare earth atoms selected from the group consisting of Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, and Yb.
  • a compound in which some or all of the free oxygen ions included in the cage are replaced with other anions include, for example, anions such as H ⁇ , H 2 ⁇ , H 2 ⁇ , O ⁇ , O 2 ⁇ , OH ⁇ , F ⁇ , Cl ⁇ , and S 2 ⁇ , and nitrogen (N). There are anions.
  • the first additional layer 140 composed of such an amorphous oxide electride is particularly referred to as an “electride layer”.
  • the electride layer can be used as an electron transport layer, an electron injection layer, and / or a hole block layer.
  • the method for forming the electride layer is not particularly limited.
  • the electride layer may be formed by, for example, a vapor deposition method.
  • Electride layer for example, the raw material was heated at 10 -3 Pa ⁇ 10 -7 in Pa vacuum, it may be deposited.
  • the electride layer may be formed by sputtering or the like.
  • the electride layer is characterized by high conductivity, a significantly high ionization potential, and a low work function. For this reason, it becomes possible to manufacture the organic EL element 100 having better characteristics by providing the electride layer.
  • two or more layers of the electron injection layer, the electron transport layer, and the hole block layer may be disposed.
  • the first additional layer 140 is a hole blocking layer
  • an electron transport layer and / or an electron injection layer are further disposed between the first additional layer 140 and the first thin film 130 in FIG. May be.
  • an electron transport layer and / or a hole blocking layer may be further disposed on the first additional layer 140 in FIG.
  • an additional electron injection layer is disposed between the first thin film 130 and the first additional layer 140 and / or the first additional layer 140 in FIG.
  • a hole blocking layer may be further disposed on the additional layer 140.
  • Step S150 the organic light emitting layer 150 is disposed on the first additional layer 140.
  • the organic light emitting layer 150 is made of a material known as a light emitting material for an organic EL element.
  • the organic light emitting layer 150 includes, for example, epidolidine, 2,5-bis [5,7-di-t-pentyl-2-benzoxazolyl] thiophene, 2,2 ′-(1,4-phenylenedivinylene) bis.
  • the organic light emitting layer 150 may be formed by a dry process such as a vapor deposition method or a transfer method. Alternatively, the organic light emitting layer 150 may be formed by a wet process such as a spin coating method, a spray coating method, or a gravure printing method.
  • the thickness of the organic light emitting layer 150 is in the range of 1 nm to 100 nm.
  • the organic light emitting layer 150 may also be used as a hole transport layer.
  • Step S160 Next, the second additional layer 160 is disposed on the organic light emitting layer 150. Note that step S160 is not an essential process, and may be omitted if unnecessary.
  • the second additional layer 160 has at least one function of a hole injection layer, a hole transport layer, and an electron blocking layer.
  • the second additional layer 160 is selected from materials having hole injection properties.
  • the second additional layer 160 may be, for example, CuPc and starburst amine.
  • the hole injection layer is a metal oxide, for example, an oxide material comprising one or more metals selected from the group consisting of molybdenum, tungsten, rhenium, vanadium, indium, tin, zinc, gallium, titanium and aluminum. Also good.
  • the method for forming the hole injection layer is not particularly limited.
  • the hole injection layer may be formed by a dry process such as an evaporation method or a transfer method.
  • the hole injection layer may be formed by a wet process such as a spin coating method, a spray coating method, or a gravure printing method.
  • the thickness of the hole injection layer is in the range of 1 nm to 50 nm.
  • the second additional layer 160 is formed as a hole transport layer
  • the second additional layer 160 is selected from materials having hole transport properties.
  • a film forming method of the hole transport layer a conventional general film forming method can be used.
  • the hole transport layer may be, for example, an arylamine compound, an amine compound containing a carbazole group, and an amine compound containing a fluorene derivative.
  • the hole transport layer comprises 4,4′-bis [N- (naphthyl) -N-phenyl-amino] biphenyl ( ⁇ -NPD), N, N′-bis (3-methylphenyl)-( 1,1′-biphenyl) -4,4′-diamine (TPD), 2-TNATA, 4,4 ′, 4 ′′ -tris (N- (3-methylphenyl) N-phenylamino) triphenylamine (MTDATA ), 4,4′-N, N′-dicarbazole biphenyl (CBP), spiro-NPD, spiro-TPD, spiro-TAD, TNB, and the like.
  • the hole transport layer can be formed using a conventional general film formation process.
  • the thickness of the hole transport layer is in the range of 1 nm to 100 nm.
  • the second additional layer 160 is formed as an electron blocking layer
  • the second additional layer 160 is selected from materials having an electron blocking property.
  • the electron block layer may be a material having a low LUMO level, for example.
  • the electron blocking layer may be, for example, tris (phenylpyrazole) iridium (Tris (phenylpyrazole) iridium: Ir (ppz) 3)).
  • two or more layers of a hole injection layer, a hole transport layer, and an electron block layer may be disposed.
  • the second additional layer 160 is an electron blocking layer
  • a hole transport layer and / or a hole injection layer may be further disposed on the second additional layer 160 in FIG.
  • the second additional layer 160 is a hole injection layer
  • a hole transport layer and / or an electron blocking layer is further disposed between the organic light emitting layer 150 and the second additional layer 160 in FIG. Also good.
  • an electron blocking layer is further disposed between the second additional layer 160 and the organic light emitting layer 150 in FIG.
  • a hole injection layer may be further disposed on the additional layer 160.
  • Step S170 Next, the second electrode 170 is disposed on the second additional layer 160.
  • the second electrode 170 a metal or a metal oxide is usually used.
  • the material used preferably has a work function of 4 eV or more.
  • the second electrode 170 needs to be transparent.
  • the second electrode 170 may be, for example, a metal material such as aluminum, silver, tin, gold, carbon, iron, cobalt, nickel, copper, zinc, tungsten, vanadium, or an alloy of the aforementioned metals. .
  • the second electrode 170 is formed of, for example, ITO, antimony oxide (Sb 2 O 3 ), zirconium oxide (ZrO 2 ), tin oxide (SnO 2 ), zinc oxide (ZnO), or IZO (Indium Zinc).
  • Oxide Oxide
  • AZO ZnO—Al 2 O 3 : zinc oxide doped with aluminum
  • GZO ZnO—Ga 2 O 3 : zinc oxide doped with gallium
  • Nb-doped TiO 2 Nb-doped TiO 2
  • metal oxides such as IWZO (In 2 O 3 —WO 3 —ZnO: indium oxide doped with tungsten trioxide and zinc oxide).
  • the film formation method of the second electrode 170 is not particularly limited.
  • the second electrode 170 may be formed by a known film formation technique such as an evaporation method, a sputtering method, or a coating method.
  • the thickness of the second electrode 170 is in the range of 50 nm to 150 nm.
  • the thickness of the second electrode 170 is preferably in the range of 2 nm to 50 nm.
  • the organic EL element 100 as shown in FIG. 2 can be manufactured.
  • the organic EL element 100 manufactured by the first manufacturing method can exhibit better characteristics than the conventional organic EL element.
  • step S130 may be performed after step S140.
  • a gas pressure may be applied. In this way, the first thin film 130 and the first additional layer 140 can be continuously formed, so that productivity is improved.
  • the characteristics have been described by taking as an example the case where the organic EL element 100 is manufactured by the first manufacturing method.
  • the inorganic EL element may be manufactured by the first manufacturing method.
  • an inorganic light emitting layer is used instead of the organic light emitting layer 150.
  • a material suitable for the inorganic EL element is used as the configuration of each layer excluding the first thin film 130.
  • the inorganic light emitting layer CdS or CdSe quantum dots are preferably dispersed.
  • Second manufacturing method a method for manufacturing a solar cell according to an embodiment of the present invention.
  • second manufacturing method a method for manufacturing a solar cell according to an embodiment of the present invention.
  • an organic solar cell is manufactured as a solar cell will be described below as an example.
  • FIG. 3 schematically shows an example of the flow of the second manufacturing method.
  • FIG. 4 schematically shows a cross section of a solar cell manufactured by the second manufacturing method.
  • the second manufacturing method is: (A) disposing the first electrode on the substrate (step S210); (B)
  • the first electrode is made of a metal oxide containing zinc (Zn) and oxygen (O), and further comprising at least one of silicon (Si) and tin (Sn).
  • step S220 Placing the thin film 1 (step S220); (C) applying a pressure by gas to the substrate having the first electrode and the first thin film (step S230); (D) placing a first additional layer on top of the first thin film (step S240); (E) a step of placing an organic photoelectric conversion layer on top of the first additional layer (step S250); (F) Arranging the second additional layer on top of the organic photoelectric conversion layer (step S260); (G) disposing a second electrode on top of the second additional layer (step S270); In this order.
  • a first electrode (cathode) 220 for example, on a substrate 210, a first electrode (cathode) 220, a first thin film 230, a first additional layer 240, an organic photoelectric conversion layer 250, The organic solar cell 200 including the second additional layer 260 and the second electrode (anode) 270 in this order is manufactured.
  • the second manufacturing method has substantially the same configuration as the first manufacturing method.
  • the organic solar cell 200 manufactured by the second manufacturing method has substantially the same configuration as the organic EL element 100 manufactured by the first manufacturing method. is there.
  • the second manufacturing method is different in that an organic photoelectric conversion layer 250 (see FIG. 4) is installed instead of the organic light emitting layer 150 (see FIG. 2) in step S250.
  • organic photoelectric conversion layer 250 those conventionally used can be used. Moreover, what was used conventionally can be used as a formation method of the organic photoelectric converting layer 250. FIG.
  • an inorganic solar cell may be manufactured by the second manufacturing method.
  • step S250 described above an inorganic photoelectric conversion layer is used instead of the organic photoelectric conversion layer 250.
  • the material suitable for an inorganic solar cell should just be used as a structure of each layer except the 1st thin film 230. FIG.
  • Example 1 An organic EL device was manufactured by the following method.
  • a sputtering apparatus was used for manufacturing the organic EL element.
  • a chamber is connected to the sputtering apparatus, and the metal mask can be exchanged in the chamber under a pressure of 10 kPa or less.
  • a cathode was formed on the substrate.
  • a non-alkali glass substrate having a length of 30 mm, a width of 30 mm, and a thickness of 0.7 mm was used as the substrate.
  • the cathode was formed by sputtering according to the following procedure.
  • the cleaned glass substrate and metal mask were placed in the chamber of the sputtering apparatus.
  • a target for cathode film formation was placed in the chamber.
  • As the target a circular Al target having a diameter of 2 inches was used.
  • An electric power of 100 W was applied to the sputter cathode, and an Al film was formed on the glass substrate.
  • the Al film was formed into a pattern with a thickness of 80 nm, a width of 1 mm, and a length of 18 mm using a metal mask.
  • the sputtering gas during film formation was Ar, and the pressure of the sputtering gas was 0.4 Pa.
  • the first thin film was a metal oxide film containing Zn and Si.
  • the distance between the target and the glass substrate during film formation was 100 mm.
  • the sputtering gas at the time of film formation was a mixed gas of Ar and O 2 , and the pressure of the sputtering gas was 0.4 Pa.
  • the Ar flow rate was 39.9 sccm, and the O 2 flow rate was 0.1 sccm.
  • the RF plasma power was 100W.
  • the film thickness was 40 nm.
  • a photoresist (S9912G) was applied on the first thin film using a spin coater. Specifically, after first applying a photoresist at 500 rpm for 5 seconds, a photoresist was further applied at 4000 rpm for 20 seconds.
  • the substrate was heated on a hot plate at 100 ° C. for 1 minute to adhere the photoresist to the first thin film.
  • the photoresist was exposed using an exposure device so that a desired pattern was obtained. Thereafter, the photoresist was developed for 40 seconds using a developer (CD26: Shipley Co., Ltd.), and unnecessary photoresist portions were removed.
  • the substrate was again heated on a hot plate at 100 ° C. for 1 minute to re-adhere the photoresist to the first thin film.
  • the substrate was immersed in an aqueous 0.01 mol / liter sodium dihydrogen tetraacetate solution (manufactured by Kanto Chemical) for 2.5 minutes to etch the exposed first thin film. Thereafter, the substrate was washed with pure water and dried by air blowing.
  • the substrate was immersed in a resist remover 104 (manufactured by Tokyo Ohka Kogyo Co., Ltd.) heated to 70 ° C. for 3 minutes, and further immersed in a resist remover 104 at 25 ° C. for 1 minute to remove the resist. Thereafter, the substrate was immersed in isopropyl alcohol for 1 minute to dry the substrate.
  • a resist remover 104 manufactured by Tokyo Ohka Kogyo Co., Ltd.
  • a patterned first thin film having a width of 1 mm and a length of 15 mm was formed on the Al film.
  • the first additional layer was an amorphous oxide electride layer containing Ca and Al, and was formed by sputtering.
  • As the target crystalline C12A7 electride was used.
  • the film formation conditions were RF power of 100 W, Ar as a film forming gas, and a total pressure of 0.1 Pa.
  • the molar ratio of Ca atoms to Al atoms is 12:14.
  • the film thickness was 5 nm.
  • Ir (ppy) 3 tris (2-phenylpyridinato) iridium (III)
  • CBP 4,4′-di (9H-carbazol-9-yl
  • Ir (ppy) 3 in the layer was 6% by weight.
  • the film thickness of the organic light emitting layer was 15 nm.
  • CBP hole transport layer
  • mobdenum oxide hole injection layer
  • a 20 nm Au layer was formed as an anode by vapor deposition.
  • the Au layer was formed as a pattern having a width of 1 mm and a length of 20 mm.
  • sample 1 an organic EL element having a light emitting region of 1 mm ⁇ (hereinafter referred to as “sample 1”) was manufactured.
  • Example 2 An organic EL device was produced in the same manner as in Example 1.
  • Example 2 after the exposure of the first thin film to the atmosphere and patterning, the substrate was placed in the chamber of the above-described sputtering apparatus and plasma treatment was performed.
  • Ar plasma was used for the plasma.
  • the Ar flow rate was 20 sccm and the pressure was 0.6 Pa.
  • the distance between the plasma cathode and the substrate was 100 mm.
  • the RF plasma power was 50W.
  • example 2 an organic EL element (hereinafter referred to as “sample 2”) was manufactured.
  • Example 3 An organic EL device was produced in the same manner as in Example 1.
  • Example 3 after the formation of the first thin film, the first additional layer was formed without taking out the substrate from the chamber, and after the formation of the first additional layer, exposure to the atmosphere was performed. Thereafter, the substrate was placed again in the chamber, and an organic light emitting layer, a hole transport layer, a hole injection layer, and an anode were formed on the first additional layer. As a result, an organic EL element (hereinafter referred to as “sample 3”) having a light emitting region of 1 mm ⁇ was manufactured.
  • the first thin film was patterned using a metal mask, and the size of the pattern was 1 mm ⁇ 15 mm.
  • Example 4 An organic EL device was produced in the same manner as in Example 1.
  • Example 4 the first thin film was not exposed to the atmosphere and patterned after the formation of the first thin film. That is, in Example 4, after the first thin film was formed, the first additional layer was formed and the subsequent steps were performed without removing the substrate from the chamber.
  • example 4 an organic EL element (hereinafter referred to as “sample 4”) was manufactured.
  • a current voltmeter (Keithley 6430) was used, and for luminance evaluation, a color luminance meter (Topcon BM-7) was used. All measurements were carried out in a UNICO glove box equipped with a circulating purifier. The atmosphere in the glove box was nitrogen.
  • Fig. 5 shows the evaluation results of Examples 1 to 4.
  • the horizontal axis represents the applied voltage
  • the vertical axis represents the light emission luminance of the sample.
  • Organic Electroluminescence Element 110 Substrate 120 First Electrode (Cathode) 130 1st thin film 140 1st additional layer 150 Organic light emitting layer 160 2nd additional layer 170 2nd electrode (anode) 200 Organic Solar Cell 210 Substrate 220 First Electrode (Cathode) 230 1st thin film 240 1st additional layer 250 Organic photoelectric conversion layer 260 2nd additional layer 270 2nd electrode (anode)

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Abstract

La présente invention porte sur un procédé de fabrication d'élément de conversion photoélectrique, ledit procédé comprenant : une étape dans laquelle une première électrode est positionnée sur un substrat ; une étape dans laquelle un premier film mince est positionné au-dessus de la première électrode, ledit premier film mince étant formé à partir d'un oxyde métallique qui comprend du zinc (Zn) et de l'oxygène (O) et comprend en outre du silicium (Si) et/ou de l'étain (Sn) ; une étape dans laquelle une pression est appliquée sur le substrat par un gaz, ledit substrat ayant la première électrode et le premier film mince ; une étape dans laquelle une couche de conversion photoélectrique est positionnée au-dessus du premier film mince, ladite couche de conversion photoélectrique étant une couche qui convertit une tension appliquée en lumière ou une couche qui convertit une lumière incidente en électricité ; et une étape dans laquelle une seconde électrode est positionnée au-dessus de la couche de conversion photoélectrique.
PCT/JP2016/084475 2015-11-30 2016-11-21 Procédé de fabrication d'élément de conversion photoélectrique WO2017094547A1 (fr)

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