WO2020085514A1 - Composition, film, structure de stratifié, dispositif électroluminescent et dispositif d'affichage - Google Patents

Composition, film, structure de stratifié, dispositif électroluminescent et dispositif d'affichage Download PDF

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WO2020085514A1
WO2020085514A1 PCT/JP2019/042100 JP2019042100W WO2020085514A1 WO 2020085514 A1 WO2020085514 A1 WO 2020085514A1 JP 2019042100 W JP2019042100 W JP 2019042100W WO 2020085514 A1 WO2020085514 A1 WO 2020085514A1
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group
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carbon atoms
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composition
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翔太 内藤
瑞穂 杉内
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住友化学株式会社
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Priority claimed from JP2019130562A external-priority patent/JP7340373B2/ja
Application filed by 住友化学株式会社 filed Critical 住友化学株式会社
Priority to CN201980069919.7A priority Critical patent/CN112930383B/zh
Priority to US17/288,424 priority patent/US20210380874A1/en
Priority to KR1020217011940A priority patent/KR20210087024A/ko
Publication of WO2020085514A1 publication Critical patent/WO2020085514A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • 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
    • H05B33/02—Details
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus

Definitions

  • the present invention relates to a composition, a film, a laminated structure, a light emitting device and a display.
  • the present application claims priority based on Japanese Patent Application No. 2018-202355 filed in Japan on October 26, 2018 and Japanese Patent Application No. 2019-130562 filed on July 12, 2019 in Japan, and The contents are incorporated here.
  • Non-Patent Document 1 a composition containing two types of inorganic luminescent particles has been reported.
  • Non-Patent Document 1 When the composition disclosed in Non-Patent Document 1 is used as a light emitting material, it is required that the emission intensity does not easily decrease.
  • the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a composition having a luminescent property in which the luminescence intensity is less likely to decrease. Another object is to provide a film, a laminated structure, a light emitting device and a display formed by using the composition.
  • the embodiment of the present invention includes the following inventions [1] to [9].
  • [1] Having a luminescent property including the component (1), the component (2), and at least one component selected from the group consisting of the component (3), the component (4), and the component (4-1).
  • Component A perovskite compound containing A, B, and X as constituent components. (A is a component located at each vertex of a hexahedron centered on B in the perovskite type crystal structure, and is a monovalent cation.
  • X represents a component located at each vertex of an octahedron centered on B in the perovskite type crystal structure, and is at least one anion selected from the group consisting of a halide ion and a thiocyanate ion.
  • B is a component located at the center of a hexahedron having A at its apex and an octahedron having X at its apex in the perovskite crystal structure, and is a metal ion.
  • Component C l N m H compound represented by n, C l N m H ions or C l of the compound represented by n N m H ion salts of the compounds represented by n (l, m And n each independently represent an integer.)
  • a perovskite compound containing A, B, and X as constituent components (A is a component located at each vertex of a hexahedron centered on B in the perovskite type crystal structure, and is a monovalent cation.
  • X represents a component located at each vertex of an octahedron centered on B in the perovskite type crystal structure, and is at least one anion selected from the group consisting of a halide ion and a thiocyanate ion.
  • Component B is a component located at the center of a hexahedron having A at its apex and an octahedron having X at its apex in the perovskite crystal structure, and is a metal ion.
  • Component The composition according to [1] or [2], which further comprises the light emitting semiconductor material [3] and the component (6).
  • Component (6) silazane, modified silazane, compound represented by the following formula (C1), modified product of compound represented by the following formula (C1), compound represented by the following formula (C2), below A modified product of the compound represented by formula (C2), a compound represented by the following formula (A5-51), a modified product of the compound represented by the following formula (A5-51), and a compound represented by the following formula (A5-52) ), A modified compound of the compound represented by the following formula (A5-52), sodium silicate, and a modified compound of sodium silicate.
  • Y 5 represents a single bond, an oxygen atom or a sulfur atom.
  • R 30 and R 31 are each independently a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or 2 carbon atoms. It represents up to 20 unsaturated hydrocarbon groups.
  • R 30 is an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or an unsaturated hydrocarbon group having 2 to 20 carbon atoms.
  • R 31 represents a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or an unsaturated hydrocarbon group having 2 to 20 carbon atoms.
  • R 30 , R 31 and R 32 each independently represent a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or a carbon atom having 3 to 30 carbon atoms. It represents 2 to 20 unsaturated hydrocarbon groups.
  • the hydrogen atoms contained in the alkyl group, cycloalkyl group and unsaturated hydrocarbon group represented by R 30 , R 31 and R 32 may be independently substituted with a halogen atom or an amino group.
  • a is an integer of 1 to 3.
  • a plurality of Y 5 s may be the same or different.
  • a plurality of R 30's may be the same or different.
  • a plurality of R 32's may be the same or different.
  • a plurality of R 31's may be the same or different.
  • a C represents a divalent hydrocarbon group
  • Y 15 represents an oxygen atom or a sulfur atom.
  • R 122 and R 123 each independently represent a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, or a cycloalkyl group having 3 to 30 carbon atoms
  • R 124 is an alkyl group having 1 to 20 carbon atoms.
  • R 125 and R 126 each independently represent a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, an alkoxy group having 1 to 20 carbon atoms, Alternatively, it represents a cycloalkyl group having 3 to 30 carbon atoms.
  • the hydrogen atoms contained in the alkyl group and cycloalkyl group represented by R 122 to R 126 may be each independently substituted with a halogen atom or an amino group.
  • Component (5) Ammonium ion, amine, primary to quaternary ammonium cation, ammonium salt, carboxylic acid, carboxylate ion, carboxylate salt, compounds represented by formulas (X1) to (X6), and At least one compound or ion selected from the group consisting of salts of compounds represented by formulas (X2) to (X4).
  • R 18 to R 21 each independently represents an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or an aryl group having 6 to 30 carbon atoms. , They may have a substituent, and M ⁇ represents a counter anion.
  • a 1 represents a single bond or an oxygen atom.
  • R 22 represents an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or an aryl group having 6 to 30 carbon atoms, which may have a substituent.
  • a 2 and A 3 each independently represent a single bond or an oxygen atom.
  • R 23 and R 24 each independently represent an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or an aryl group having 6 to 30 carbon atoms, each of which has a substituent. You may have.
  • a 4 represents a single bond or an oxygen atom.
  • R 25 represents an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or an aryl group having 6 to 30 carbon atoms, which may have a substituent.
  • a 5 to A 7 each independently represent a single bond or an oxygen atom.
  • R 26 to R 28 are each independently an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, an aryl group having 6 to 30 carbon atoms, an alkenyl group having 2 to 20 carbon atoms. Or represents an alkynyl group having 2 to 20 carbon atoms, which may have a substituent.
  • a 8 to A 10 each independently represent a single bond or an oxygen atom.
  • R 29 to R 31 are each independently an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, an aryl group having 6 to 30 carbon atoms, an alkenyl group having 2 to 20 carbon atoms. Or represents an alkynyl group having 2 to 20 carbon atoms, which may have a substituent.
  • the hydrogen atoms contained in the groups represented by R 18 to R 31 may each independently be substituted with a halogen atom.
  • Component (5-1) At least one compound or ion selected from the group consisting of ammonium ions, amines, primary to quaternary ammonium cations, ammonium salts, carboxylic acids, carboxylate ions, and carboxylate salts.
  • a film comprising the composition according to any one of [1] to [5] as a forming material.
  • a laminated structure including the film according to [6].
  • a light emitting device including the laminated structure according to [7].
  • a display including the laminated structure according to [7].
  • the present invention it is possible to provide a composition, a film, a laminated structure, a light emitting device, and a display which have a light emitting property and whose emission intensity is unlikely to decrease.
  • the composition of this embodiment has a light emitting property.
  • Luminescent refers to the property of emitting light.
  • the light emitting property is preferably a property of emitting light when excited by an electron, and more preferably a property of emitting light when excited by an electron by excitation light.
  • the wavelength of the excitation light may be, for example, 200 nm to 800 nm, 250 nm to 750 nm, or 300 nm to 700 nm.
  • the first aspect of the composition of the present embodiment is at least one selected from the group consisting of component (1), component (2), component (3), component (4), and component (4-1).
  • a composition having a luminescent property is at least one selected from the group consisting of component (1), component (2), component (3), component (4), and component (4-1).
  • a composition having a luminescent property The molar ratio of nitrogen atoms contained in the component (2) to B contained in the component (1) exceeds 0 and is 0.55.
  • Component A perovskite compound containing A, B, and X as constituent components.
  • A is a component located at each vertex of a hexahedron centered on B in the perovskite type crystal structure, and is a monovalent cation.
  • X represents a component located at each vertex of an octahedron centered on B in the perovskite type crystal structure, and is at least one anion selected from the group consisting of a halide ion and a thiocyanate ion.
  • B is a component located at the center of a hexahedron having A at its apex and an octahedron having X at its apex in the perovskite crystal structure, and is a metal ion.
  • component C l N m H compound represented by n, C l N m H ions or C l of the compound represented by n N m H ion salts of the compounds represented by n (l, m And n each independently represent an integer.)
  • the above-mentioned other embodiment is a light emission containing the component (1), the component (2), and at least one component selected from the group consisting of the component (3), the component (4), and the component (4-1). It is a composition having properties.
  • the content of nitrogen atoms contained in the component (2) is 7600 mass ppm or less based on the total mass of the composition.
  • Component A perovskite compound containing A, B, and X as constituent components.
  • component C l N m H compound represented by n, C l N m H ions or C l of the compound represented by n N m H ion salts of the compounds represented by n (l, m , And n each independently represent an integer.)
  • the component (1) may be referred to as the (1) perovskite compound.
  • the component (2) may be referred to as the (2) amine compound group.
  • (3) solvent, (4) polymerizable compound, and (4-1) polymer may be collectively referred to as “dispersion medium”.
  • the composition of the present embodiment may be dispersed in these dispersion media.
  • dispersed means (1) a state where the perovskite compound is suspended in the dispersion medium, or (1) a state where the perovskite compound is suspended in the dispersion medium.
  • a part of the (1) perovskite compound may be precipitated.
  • Perovskite compound has a perovskite type crystal structure having A, B and X as constituent components.
  • a compound semiconductor having a perovskite structure may be simply referred to as “perovskite compound”.
  • A is a component located at each vertex of a hexahedron centered on B and is a monovalent cation.
  • B is a component located at the center of the hexahedron having A at its apex and the octahedron having X at its apex, and is a metal ion.
  • B is a metal cation capable of adopting the octahedral coordination of X.
  • X represents a component located at each vertex of the octahedron centered on B in the perovskite type crystal structure, and is at least one anion selected from the group consisting of a halide ion and a thiocyanate ion.
  • the perovskite compound having A, B, and X as constituent components is not particularly limited, and may be a compound having any of a three-dimensional structure, a two-dimensional structure, and a pseudo two-dimensional (quasi-2D) structure.
  • the composition formula of the perovskite compound is represented by ABX (3 + ⁇ ) .
  • the composition formula of the perovskite compound is represented by A 2 BX (4 + ⁇ ) .
  • ⁇ is a number that can be appropriately changed according to the charge balance of B, and is ⁇ 0.7 or more and 0.7 or less.
  • A is a monovalent cation
  • B is a divalent cation
  • X is a monovalent anion
  • ⁇ can be selected so that the perovskite compound becomes electrically neutral.
  • the electrically neutral perovskite compound means that the charge of the perovskite compound is zero.
  • the perovskite compound includes an octahedron whose center is B and whose apex is X.
  • the octahedron is represented by BX 6 . If perovskite compound has a 3-dimensional structure, BX 6 contained in the perovskite compound, share one X is located at the apex in octahedral (BX 6), 2 octahedral adjacent in the crystal (BX 6) By doing so, a three-dimensional network is constructed.
  • perovskite compound has a two-dimensional structure, BX 6 contained in the perovskite compound, shared by the two X located at the vertices in octahedral (BX 6), 2 octahedral adjacent in the crystal (BX 6) By doing so, the ridgeline of the octahedron is shared and a two-dimensionally continuous layer is formed.
  • the perovskite compound has a structure in which two-dimensionally continuous layers of BX 6 and layers of A are alternately laminated.
  • the crystal structure of the perovskite compound can be confirmed by an X-ray diffraction pattern.
  • the perovskite compound preferably has a three-dimensional structure.
  • a constituting the perovskite compound is a monovalent cation.
  • Examples of A include cesium ion, organic ammonium ion, and amidinium ion.
  • organic ammonium ion Specific examples of the organic ammonium ion of A include a cation represented by the following formula (A3).
  • R 6 to R 9 each independently represent a hydrogen atom, an alkyl group, or a cycloalkyl group. However, at least one of R 6 to R 9 is an alkyl group or a cycloalkyl group, and all of R 6 to R 9 are not hydrogen atoms at the same time.
  • the alkyl group represented by R 6 to R 9 may be linear or branched.
  • the alkyl groups represented by R 6 to R 9 may each independently have an amino group as a substituent.
  • R 6 to R 9 are each an alkyl group
  • the number of carbon atoms is independently 1 to 20, usually 1 to 4, preferably 1 to 3, and more preferably 1. Is more preferable.
  • the cycloalkyl groups represented by R 6 to R 9 may each independently have an amino group as a substituent.
  • the number of carbon atoms of the cycloalkyl group represented by R 6 to R 9 is, independently of each other, usually 3 to 30, preferably 3 to 11, and more preferably 3 to 8.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • the groups represented by R 6 to R 9 are preferably each independently a hydrogen atom or an alkyl group.
  • the perovskite compound contains, as A, an organic ammonium ion represented by the above formula (A3)
  • A an organic ammonium ion represented by the above formula (A3)
  • the number of alkyl groups and cycloalkyl groups contained in the formula (A3) be small.
  • the number of carbon atoms of the alkyl group and the cycloalkyl group which can be included in the formula (A3) is preferably small. Thereby, a perovskite compound having a three-dimensional structure with high emission intensity can be obtained.
  • the total number of carbon atoms contained in the alkyl group and cycloalkyl group represented by R 6 to R 9 is preferably 1 to 4.
  • one of R 6 ⁇ R 9 is an alkyl group having 1 to 3 carbon atoms
  • three of R 6 ⁇ R 9 is a hydrogen atom More preferably.
  • the alkyl group of R 6 to R 9 is a methyl group, an ethyl group, an n-propyl group, an isopropyl group, an n-butyl group, an isobutyl group, a sec-butyl group, a tert-butyl group, an n-pentyl group, an isopentyl group.
  • the cycloalkyl group of R 6 ⁇ R 9, include those independently R 6 ⁇ exemplified alkyl group having 3 or more carbon atoms in the alkyl group R 9 is to form a ring.
  • Examples include cyclopropyl group, cyclobutyl group, cyclopentyl group, cyclohexyl group, cycloheptyl group, cyclooctyl group, cyclononyl group, cyclodecyl group, norbornyl group, isobornyl group, 1-adamantyl group, 2-adamantyl group, tricyclodecyl group.
  • Etc. can be illustrated.
  • Examples of the organic ammonium ion represented by A include CH 3 NH 3 + (also called methylammonium ion), C 2 H 5 NH 3 + (also called ethylammonium ion) or C 3 H 7 NH 3 + (propyl). It is also preferably an ammonium ion), more preferably CH 3 NH 3 + or C 2 H 5 NH 3 + , and further preferably CH 3 NH 3 + .
  • amidinium ion examples include an amidinium ion represented by the following formula (A4).
  • R 10 R 11 N CH—NR 12 R 13 ) + ...
  • R 10 to R 13 are each independently a hydrogen atom, an alkyl group which may have an amino group as a substituent, or a cycloalkyl which may have an amino group as a substituent. Represents a group.
  • the alkyl groups represented by R 10 to R 13 may each independently be linear or branched.
  • the alkyl groups represented by R 10 to R 13 may each independently have an amino group as a substituent.
  • the number of carbon atoms of the alkyl group represented by R 10 to R 13 is independently 1 to 20, usually 1 to 4, and more preferably 1 to 3.
  • the cycloalkyl groups represented by R 10 to R 13 may each independently have an amino group as a substituent.
  • the number of carbon atoms of the cycloalkyl group represented by R 10 to R 13 is, independently of each other, usually 3 to 30, preferably 3 to 11, and more preferably 3 to 8.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • alkyl group of R 10 to R 13 include the same groups as the alkyl groups exemplified in R 6 to R 9 each independently.
  • cycloalkyl group of R 10 to R 13 include the same groups as the cycloalkyl group exemplified in R 6 to R 9 each independently.
  • the groups represented by R 10 to R 13 are preferably each independently a hydrogen atom or an alkyl group.
  • the total number of carbon atoms contained in the alkyl group and cycloalkyl group represented by R 10 to R 13 is preferably 1 to 4, and R 10 is an alkyl group having 1 carbon atom. It is more preferable that R 11 to R 13 are hydrogen atoms.
  • the perovskite compound when A is a cesium ion, an organic ammonium ion having 3 or less carbon atoms, or an amidinium ion having 3 or less carbon atoms, the perovskite compound generally has a three-dimensional structure.
  • the perovskite compound when A is an organic ammonium ion having 4 or more carbon atoms or an amidinium ion having 4 or more carbon atoms, the perovskite compound has either a two-dimensional structure or a pseudo two-dimensional (quasi-2D) structure. Have one or both. In this case, the perovskite compound can have a two-dimensional structure or a pseudo-two-dimensional structure in a part or the whole of the crystal. When a plurality of two-dimensional perovskite type crystal structures are laminated, it becomes equivalent to a three-dimensional perovskite type crystal structure (references: P. PBoix et al., J. Phys. Chem. Lett. 2015, 6, 898-907, etc.).
  • a in the perovskite compound is preferably a cesium ion or an amidinium ion.
  • the amidinium ions a formamidinium ion in which R 10 to R 13 are all hydrogen atoms is preferable.
  • Component B constituting the perovskite compound may be one or more kinds of metal ions selected from the group consisting of monovalent metal ions, divalent metal ions, and trivalent metal ions.
  • B preferably contains a divalent metal ion, more preferably contains at least one metal ion selected from the group consisting of lead and tin, and even more preferably lead.
  • Component X constituting the perovskite compound may be at least one anion selected from the group consisting of a halide ion and a thiocyanate ion.
  • halide ion chloride ion, bromide ion, fluoride ion, iodide ion can be mentioned.
  • X is preferably a bromide ion.
  • the content ratio of halide ions can be appropriately selected according to the emission wavelength.
  • a combination of bromide ion and chloride ion or a combination of bromide ion and iodide ion can be used.
  • X can be appropriately selected according to the desired emission wavelength.
  • a perovskite compound in which X is a bromide ion can emit fluorescence having a maximum intensity peak in a wavelength range of usually 480 nm or more, preferably 500 nm or more, more preferably 520 nm or more.
  • the perovskite compound in which X is a bromide ion can emit fluorescence having a maximum intensity peak in a wavelength range of usually 700 nm or less, preferably 600 nm or less, more preferably 580 nm or less.
  • the upper limit value and the lower limit value of the above wavelength range can be arbitrarily combined.
  • the peak of fluorescence emitted is usually 480 to 700 nm, preferably 500 to 600 nm, and more preferably 520 to 580 nm.
  • the perovskite compound in which X is an iodide ion can emit fluorescence having a maximum intensity peak in a wavelength range of usually 520 nm or more, preferably 530 nm or more, more preferably 540 nm or more.
  • a perovskite compound in which X is an iodide ion can emit fluorescence having a maximum intensity peak in a wavelength range of usually 800 nm or less, preferably 750 nm or less, more preferably 730 nm or less.
  • the upper limit value and the lower limit value of the above wavelength range can be arbitrarily combined.
  • the fluorescence peak emitted is usually 520 to 800 nm, preferably 530 to 750 nm, and more preferably 540 to 730 nm.
  • a perovskite compound in which X is a chloride ion can emit fluorescence having a maximum intensity peak in a wavelength range of usually 300 nm or more, preferably 310 nm or more, more preferably 330 nm or more.
  • the perovskite compound in which X is a chloride ion can emit fluorescence having a maximum intensity peak in a wavelength range of usually 600 nm or less, preferably 580 nm or less, and more preferably 550 nm or less.
  • the upper limit value and the lower limit value of the above wavelength range can be arbitrarily combined.
  • the peak of fluorescence emitted is usually 300 to 600 nm, preferably 310 to 580 nm, and more preferably 330 to 550 nm.
  • the perovskite compound having a three-dimensional structure examples include CH 3 NH 3 Pb (1-a) Ca a Br 3 (0 ⁇ a ⁇ 0.7), CH 3 NH 3 Pb (1-a) Sr a Br 3 (0 ⁇ a ⁇ 0.7), CH 3 NH 3 Pb (1-a) La a Br (3 + ⁇ ) (0 ⁇ a ⁇ 0.7, 0 ⁇ ⁇ 0.7), CH 3 NH 3 Pb ( 1-a) Ba a Br 3 (0 ⁇ a ⁇ 0.7), CH 3 NH 3 Pb (1-a) Dy a Br (3 + ⁇ ) (0 ⁇ a ⁇ 0.7, 0 ⁇ ⁇ 0.7 ) Can also be mentioned.
  • Preferred examples of the three-dimensional perovskite compound include CH 3 NH 3 Pb (1-a) Na a Br (3 + ⁇ ) (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ ⁇ 0), CH 3 NH 3 Pb (1-a) Li a Br (3 + ⁇ ) (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ ⁇ 0) can also be mentioned.
  • Preferred examples of the three-dimensional perovskite compound include CsPb (1-a) Na a Br (3 + ⁇ ) (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ ⁇ 0) and CsPb (1-a) Li. There can also be mentioned a Br (3 + ⁇ ) (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ ⁇ 0).
  • the three-dimensional perovskite compound include CH 3 NH 3 Pb (1-a) Na a Br (3 + ⁇ y) I y (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ ⁇ 0, 0 ⁇ y ⁇ 3), CH 3 NH 3 Pb (1-a) Li a Br (3 + ⁇ y) I y (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ ⁇ 0, 0 ⁇ y ⁇ 3 ), CH 3 NH 3 Pb (1-a) Na a Br (3 + ⁇ y) Cl y (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ ⁇ 0, 0 ⁇ y ⁇ 3), CH 3 NH 3 Pb (1-a) Li a Br (3 + ⁇ -y) Cl y (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ ⁇ 0, 0 ⁇ y ⁇ 3) can also be mentioned.
  • Preferred examples of the three-dimensional perovskite compound include CsPbBr 3 , CsPbCl 3 , CsPbI 3 , CsPbBr (3-y) I y (0 ⁇ y ⁇ 3), CsPbBr (3-y) Cl y (0 ⁇ y ⁇ 3) can also be mentioned.
  • Preferred examples of the perovskite compound having a three-dimensional structure include CH 3 NH 3 Pb (1-a) Zn a Br 3 (0 ⁇ a ⁇ 0.7), CH 3 NH 3 Pb (1-a) Al a Br ( 3 + ⁇ ) (0 ⁇ a ⁇ 0.7, 0 ⁇ ⁇ ⁇ 0.7), CH 3 NH 3 Pb (1-a) Co a Br 3 (0 ⁇ a ⁇ 0.7), CH 3 NH 3 Pb ( 1-a) Mn a Br 3 (0 ⁇ a ⁇ 0.7) and CH 3 NH 3 Pb (1-a) Mg a Br 3 (0 ⁇ a ⁇ 0.7) can also be mentioned.
  • Preferred examples of perovskite compound having a three-dimensional structure is, CsPb (1-a) Zn a Br 3 (0 ⁇ a ⁇ 0.7), CsPb (1-a) Al a Br (3 + ⁇ ) (0 ⁇ a ⁇ 0 .7, 0 ⁇ ⁇ 0.7), CsPb (1-a) Co a Br 3 (0 ⁇ a ⁇ 0.7), CsPb (1-a) Mna a Br 3 (0 ⁇ a ⁇ 0.7) ) And CsPb (1-a) Mg a Br 3 (0 ⁇ a ⁇ 0.7) can also be mentioned.
  • Preferred examples of the three-dimensional perovskite compound are CH 3 NH 3 Pb (1-a) Zn a Br (3-y) I y (0 ⁇ a ⁇ 0.7, 0 ⁇ y ⁇ 3), CH 3 NH 3 Pb (1-a) Al a Br (3 + ⁇ -y) I y (0 ⁇ a ⁇ 0.7,0 ⁇ ⁇ 0.7,0 ⁇ y ⁇ 3), CH 3 NH 3 Pb (1- a) Co a Br (3- y) I y (0 ⁇ a ⁇ 0.7,0 ⁇ y ⁇ 3), CH 3 NH 3 Pb (1-a) Mn a Br (3-y) I y (0 ⁇ A ⁇ 0.7, 0 ⁇ y ⁇ 3), CH 3 NH 3 Pb (1-a) Mg a Br (3-y) I y (0 ⁇ a ⁇ 0.7, 0 ⁇ y ⁇ 3), CH 3 NH 3 Pb (1-a) Zn a Br (3-y) Cl y (0
  • CsPbBr 3 , CsPbBr (3-y) I y (0 ⁇ y ⁇ 3), and (H 2 N CH—NH 2 ) PbBr 3 are more preferable, and (H 2 N Further preferred is ⁇ CH—NH 2 ) PbBr 3 .
  • Preferred examples of the perovskite compound having a two-dimensional structure include (C 4 H 9 NH 3 ) 2 PbBr 4 , (C 4 H 9 NH 3 ) 2 PbCl 4 , (C 4 H 9 NH 3 ) 2 PbI 4 , and (C 7 H 15 NH 3 ) 2 PbBr 4 , (C 7 H 15 NH 3 ) 2 PbCl 4 , (C 7 H 15 NH 3 ) 2 PbI 4 , (C 4 H 9 NH 3 ) 2 Pb (1-a) Li a Br (4 + ⁇ ) (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ 0), (C 4 H 9 NH 3 ) 2 Pb (1-a) Na a Br (4 + ⁇ ) (0 ⁇ a ⁇ 0.7, ⁇ 0.7 ⁇ ⁇ 0), (C 4 H 9 NH 3 ) 2 Pb (1-a)
  • Preferable examples of the two-dimensional perovskite compound also include (C 4 H 9 NH 3 ) 2 PbBr 4 and (C 7 H 15 NH 3 ) 2 PbBr 4 .
  • Preferred examples of the two-dimensional perovskite compound include (C 4 H 9 NH 3 ) 2 PbBr (4-y) Cl y (0 ⁇ y ⁇ 4), (C 4 H 9 NH 3 ) 2 PbBr (4- y) I y (0 ⁇ y ⁇ 4) can also be mentioned.
  • the perovskite compound having a two-dimensional structure examples include (C 4 H 9 NH 3 ) 2 Pb (1-a) Zn a Br 4 (0 ⁇ a ⁇ 0.7), (C 4 H 9 NH 3 ) 2 Pb (1-a) Mg a Br 4 (0 ⁇ a ⁇ 0.7), (C 4 H 9 NH 3 ) 2 Pb (1-a) Co a Br 4 (0 ⁇ a ⁇ 0.7), ( C 4 H 9 NH 3) 2 Pb (1-a) Mn a Br 4 (0 ⁇ a ⁇ 0.7) may also be mentioned.
  • the perovskite compound having a two-dimensional structure examples include (C 7 H 15 NH 3 ) 2 Pb (1-a) Zn a Br 4 (0 ⁇ a ⁇ 0.7), (C 7 H 15 NH 3 ) 2 Pb (1-a) Mg a Br 4 (0 ⁇ a ⁇ 0.7), (C 7 H 15 NH 3 ) 2 Pb (1-a) Co a Br 4 (0 ⁇ a ⁇ 0.7), ( C 7 H 15 NH 3) 2 Pb (1-a) Mn a Br 4 (0 ⁇ a ⁇ 0.7) may also be mentioned.
  • the average particle size of the perovskite compound is not particularly limited, but is preferably 1 nm or more because the crystal structure can be maintained well.
  • the average particle size of the perovskite compound is more preferably 2 nm or more, further preferably 3 nm or more.
  • the average particle size of the perovskite compound is preferably 10 ⁇ m or less because it is easy to maintain desired emission characteristics.
  • the average particle size of the perovskite compound is more preferably 1 ⁇ m or less, further preferably 500 nm or less.
  • emission characteristic refers to optical properties such as quantum yield, emission intensity, and color purity of converted light obtained by irradiating a perovskite compound with excitation light. The color purity can be evaluated by the full width at half maximum of the spectrum of converted light.
  • the upper limit value and the lower limit value of the average particle diameter of the perovskite compound can be arbitrarily combined.
  • the average particle size of the perovskite compound is preferably 1 nm or more and 10 ⁇ m or less, more preferably 2 nm or more and 1 ⁇ m or less, and further preferably 3 nm or more and 500 nm or less.
  • the average particle size of the perovskite compound can be measured by, for example, a transmission electron microscope (hereinafter also referred to as TEM) or a scanning electron microscope (hereinafter also referred to as SEM).
  • TEM transmission electron microscope
  • SEM scanning electron microscope
  • the average particle diameter can be determined by measuring the maximum Feret diameter of 20 perovskite compounds by TEM or SEM and calculating the average maximum Feret diameter that is the arithmetic mean value of the measured values.
  • the “maximum Feret diameter” means the maximum distance between two parallel straight lines sandwiching a perovskite compound on a TEM or SEM image.
  • the median diameter (D50) of the perovskite compound is not particularly limited, but is preferably 3 nm or more because the crystal structure can be maintained well.
  • the median diameter of the perovskite compound is more preferably 4 nm or more, further preferably 5 nm or more.
  • the median diameter (D50) of the perovskite compound is preferably 5 ⁇ m or less because it is easy to maintain desired emission characteristics.
  • the median diameter of the perovskite compound is more preferably 500 nm or less, further preferably 100 nm or less.
  • the upper limit and the lower limit of the median diameter (D50) of the perovskite compound can be arbitrarily combined.
  • the median diameter (D50) of the perovskite compound is preferably 3 nm or more and 5 ⁇ m or less, more preferably 4 nm or more and 500 nm or less, and further preferably 5 nm or more and 100 nm or less.
  • the particle size distribution of the perovskite compound can be measured by, for example, TEM or SEM. Specifically, the maximum Feret diameter of 20 perovskite compounds is observed by TEM or SEM, and the median diameter (D50) can be obtained from the distribution of the maximum Feret diameter.
  • perovskite compound only one type of perovskite compound may be used, or two or more types may be used in combination.
  • the component (A) of the (1) perovskite compound is an organic ammonium or amidinium ion, and the (1) perovskite compound and the (2) amine compound group are different components.
  • l, m, and n are each independently a positive integer. l is, for example, preferably 1 to 30, and more preferably 1 to 18.
  • n is, for example, preferably 1 to 5, more preferably 1 to 3, and further preferably 1 to 2.
  • n is preferably, for example, 4 to 60, and more preferably 4 to 40.
  • the ion of the compound represented by C 1 N m H n means, for example, that one or more protons are bound to the compound represented by C 1 N m H n and one or more N atoms are positively charged. There are ammonium ions and amidinium ions. Further, C l N m and the salt of the ionic compound represented by H n, the C l N m with respect to H n positively charged in the ion of the compound represented by the N-linked counters anion Means the compound formed.
  • the counter anion is not particularly limited, but examples thereof include Cl, Br, and I.
  • the ammonium salt represented by the formula (A1), the amidinium ion represented by the formula (A4-1), and the ion salt of the compound represented by C 1 N m H n are represented by the formula (A1) described below. ) And the salt formed by the amidinium ion represented by formula (A4-1) binding to the counter anion.
  • Examples of the (2) amine compound group in the present embodiment include C such as methylamine, ethylamine, propylamine, oleylamine, n-octylamine, nonylamine, 1-aminodecane, dodecylamine, tetradecylamine and 1-aminoheptadecane.
  • R 10 ⁇ R 13 are the same as R 10 ⁇ R 13 in the formula (A4).
  • the first aspect of the composition of the present embodiment is that the molar ratio of the nitrogen atom contained in the (2) amine compound group to the B contained in the (1) perovskite compound is (1) from the viewpoint of emission characteristics of the perovskite compound. Therefore, it is 0.55 or less, preferably 0.5 or less, more preferably 0.4 or less, and further preferably 0.3 or less.
  • the molar ratio is more than 0, may be 0.01 or more, may be 0.03 or more, may be 0.06 or more, and may be 0.1 or more. It is preferably 0.13 or more, more preferably 0.16 or more, further preferably 0.20 or more, further preferably 0.23 or more, and 0.25 or more. Is particularly preferable.
  • the upper limit value and the lower limit value can be arbitrarily combined, but are more than 0 and 0.55 or less, may be 0.01 or more and 0.5 or less, and are 0.02 or more and 0.4 or less. May be 0.03 or more and 0.3 or less, 0.06 or more and 0.3 or less, preferably 0.10 or more and 0.3 or less, and 0.13 or more It is more preferably 0.3 or less, further preferably 0.16 or more and 0.3 or less, further preferably 0.20 or more and 0.3 or less, and 0.23 or more and 0.3 or less. It is more preferable to be present, and it is particularly preferable to be 0.25 or more and 0.3 or less.
  • the molar ratio is within this range, the decrease of the emission spectrum intensity of the (1) perovskite compound contained in the composition can be suppressed, and when the composition contains (10) the luminescent semiconductor material, the composition (10) It is possible to suppress an increase in the half-value width of the peak that gives the maximum emission intensity of the emission spectrum of the light-emitting semiconductor material included in (10).
  • the emission color purity is high.
  • the content of the nitrogen atom contained in the (2) amine compound group is 7600 mass ppm or less, preferably 5000 mass ppm or less, and more preferably 2000 mass ppm or less with respect to the total mass of the composition. It is preferably 1000 mass ppm or less, more preferably 300 mass ppm or less.
  • the content of nitrogen atoms contained in the amine compound group is 0.1 mass ppm or more based on the total mass of the composition, and (1) 1 mass ppm from the viewpoint of maintaining the light emission characteristics of the perovskite compound. It is preferably at least 4 mass ppm, more preferably at least 10 mass ppm, further preferably at least 20 mass ppm, particularly preferably at least 40 mass ppm.
  • the content of nitrogen atoms contained in the amine compound group is preferably 0.1 mass ppm or more and 7600 mass ppm or less with respect to the total mass of the composition, and 1 mass ppm or more and 5000 mass ppm or less Is more preferable, 4 mass ppm or more and 2000 mass ppm or less is further preferable, 10 mass ppm or more and 1000 mass ppm or less is further preferable, and 20 mass ppm or more and 1000 mass ppm or less is further It is preferably 40 mass ppm or more and 300 mass ppm or less.
  • the composition of the present embodiment is (2) a composition in which the content of nitrogen atoms contained in the amine compound group is not more than the above upper limit value with respect to the total mass of the composition, in other words, the content of impurities is small. It is characterized by that. Due to the small amount of impurities, it is possible to suppress a decrease in emission intensity when used in combination with a semiconductor material such as indium phosphide.
  • the content of nitrogen atoms contained in the amine compound group may be about the above lower limit or more. If the amine compound group (2) contains a small amount of nitrogen atom, it acts as a surface modifier of the (1) perovskite compound, and the dispersibility of the (1) perovskite compound in the composition is improved.
  • Specific examples of the amine compound group include (1) a manufacturing residue generated in the manufacturing process of a perovskite compound and (5) a residue of a compound contained in a surface modifier contained as an optional component.
  • composition of the present embodiment contains the amine compound group, only one kind may be contained or two or more kinds may be contained in the above-mentioned amine compound group.
  • the content of the (2) amine compound group contained in the composition of the present embodiment is reduced, for example, a method of washing (1) the perovskite compound as a raw material to remove it in advance, diluting the composition, or the like is used. Can be done using.
  • the mass of nitrogen atoms contained in the amine compound group is measured by using XPS, ICP, or a gas chromatograph using a mass spectrometer (Mass Spectrometry (hereinafter, also referred to as “MS”)) as a detector. can do.
  • mass spectrometer Mass Spectrometry (hereinafter, also referred to as “MS”)
  • gas chromatographic measurement is referred to as GC-MS measurement.
  • composition of the present embodiment (2) if C l N m is represented by H n compounds contained in the amine compound group of having 2 or more, (2) an amine group of compounds, two or more amine compounds Composed of.
  • the mass of nitrogen atoms contained in the amine compound group (2) in the composition can be calculated from the total mass of nitrogen atoms contained in each amine compound group constituting the amine compound group (2).
  • the mass of nitrogen atoms contained in the (2) amine compound group in the composition is determined by, for example, the following method.
  • XPS X-ray photoelectron spectroscopy
  • the XPS measurement is preferably performed after the composition containing the perovskite is cast on a glass substrate and dried.
  • composition of the present embodiment contains at least one dispersion medium selected from the group consisting of component (3), component (4) and component (4-1).
  • component solvent (4)
  • component polymerizable compound (4-1)
  • component polymer
  • solvent is not particularly limited as long as it is a medium that can disperse the (1) perovskite compound, but a solvent that is difficult to dissolve the (1) perovskite compound is preferable.
  • solvent refers to a substance that is in a liquid state at 1 atmosphere and 25 ° C. However, the solvent does not include a polymerizable compound and a polymer described later.
  • solvent examples include the following (a) to (k).
  • Examples of (a) ester include methyl formate, ethyl formate, propyl formate, pentyl formate, methyl acetate, ethyl acetate, pentyl acetate and the like.
  • ketones examples include ⁇ -butyrolactone, N-methyl-2-pyrrolidone, acetone, diisobutyl ketone, cyclopentanone, cyclohexanone, and methylcyclohexanone.
  • ether (c) examples include diethyl ether, methyl-tert-butyl ether, diisopropyl ether, dimethoxymethane, dimethoxyethane, 1,4-dioxane, 1,3-dioxolane, 4-methyldioxolane, tetrahydrofuran, methyltetrahydrofuran, anisole and phenetole. Etc. can be mentioned.
  • glycol ethers examples include ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol monoethyl ether acetate, and triethylene glycol dimethyl ether.
  • Examples of the organic solvent having an amide group include N, N-dimethylformamide, acetamide, N, N-dimethylacetamide and the like.
  • Examples of the organic solvent having a nitrile group include acetonitrile, isobutyronitrile, propionitrile, and methoxyacetonitrile.
  • Examples of the organic solvent having a carbonate group include ethylene carbonate and propylene carbonate.
  • halogenated hydrocarbons examples include methylene chloride and chloroform.
  • Examples of the (j) hydrocarbon include n-pentane, cyclohexane, n-hexane, 1-octadecene, benzene, toluene and xylene.
  • the above solvent may be used alone or in combination of two or more.
  • the polymerizable compound contained in the composition of the present embodiment is preferably one that is difficult to dissolve the (1) perovskite compound at the temperature for producing the composition of the present embodiment.
  • the “polymerizable compound” means a monomer compound (monomer) having a polymerizable group.
  • the polymerizable compound may include a monomer that is in a liquid state at 1 atmosphere and 25 ° C.
  • the polymerizable compound when the composition is produced at room temperature under normal pressure, is not particularly limited.
  • the polymerizable compound include known polymerizable compounds such as styrene, acrylic acid ester, methacrylic acid ester, and acrylonitrile. Among them, as the polymerizable compound, one or both of acrylic acid ester and methacrylic acid ester, which are monomers of the acrylic resin, are preferable.
  • the polymerizable compound may be used alone or in combination of two or more.
  • the ratio of the total amount of acrylic acid ester and methacrylic acid ester to all (4) polymerizable compounds may be 10 mol% or more. The same ratio may be 30 mol% or more, 50 mol% or more, 80 mol% or more, and 100 mol%.
  • the polymer contained in the composition of the present embodiment is preferably a polymer having a low solubility of the (1) perovskite compound at the temperature for producing the composition of the present embodiment.
  • the polymer when it is produced at room temperature under normal pressure, is not particularly limited, and examples thereof include known polymers such as polystyrene, acrylic resin, and epoxy resin. Among them, the acrylic resin is preferable as the polymer.
  • the acrylic resin contains either one or both of a structural unit derived from an acrylate ester and a structural unit derived from a methacrylic acid ester.
  • the ratio of the total amount of the structural unit derived from the acrylate ester and the structural unit derived from the methacrylic acid ester to all the structural units contained in the (4-1) polymer is 10 mol%. It may be more than. The same ratio may be 30 mol% or more, 50 mol% or more, 80 mol% or more, and 100 mol%.
  • the weight average molecular weight of the (4-1) polymer is preferably 100 to 1200000, more preferably 1000 to 800000, and further preferably 5000 to 150,000.
  • composition of the present embodiment only one kind of polymer may be used, or two or more kinds of polymers may be used in combination.
  • the “weight average molecular weight” means a polystyrene conversion value measured by a gel permeation chromatography (GPC) method.
  • the content ratio of (1) perovskite compound to the total mass of the composition is not particularly limited.
  • the content ratio is preferably 90% by mass or less, more preferably 40% by mass or less, further preferably 10% by mass or less, and 3% by mass or less. Is particularly preferred.
  • the content ratio is preferably 0.0002 mass% or more, more preferably 0.002 mass% or more, and 0.01 mass% or more from the viewpoint of obtaining a good quantum yield. Is more preferable.
  • the content ratio of (1) perovskite compound to the total mass of the composition is usually 0.0002 to 90 mass%.
  • the content ratio of the (1) perovskite compound to the total mass of the composition is preferably 0.001 to 40% by mass, more preferably 0.002 to 10% by mass, and 0.01 to 3% by mass. Is more preferable.
  • composition in which the content ratio of the (1) perovskite compound to the total mass of the composition is within the above range is preferable in that the aggregation of the (1) perovskite compound does not easily occur and the luminescent property is exhibited well.
  • the total content of the (1) perovskite compound and the dispersion medium may be 90% by mass or more, or 95% by mass or more, relative to the total mass of the composition, 99 It may be not less than mass% or may be 100 mass%.
  • the mass ratio of the (1) perovskite compound to the dispersion medium may be 0.00001 to 10, or 0.0001 to 2. It may be 0.0005 to 1.
  • a composition in which the range of the compounding ratio of the (1) perovskite compound and the dispersion medium is within the above range is preferable in that (1) the perovskite compound is less likely to aggregate and emits light well.
  • the composition of the present embodiment is a component other than the above-mentioned (1) perovskite compound, (3) solvent, (4) polymerizable compound, and (4-1) polymer (hereinafter referred to as “other component”). ) May be included.
  • Other components include, for example, a small amount of impurities, (1) a compound having an amorphous structure composed of elemental components constituting the perovskite compound, and a polymerization initiator.
  • the content ratio of the other components is preferably 10% by mass or less, more preferably 5% by mass or less, and further preferably 1% by mass or less, based on the total mass of the composition.
  • the above-mentioned (4-1) polymer can be adopted.
  • the (1) perovskite compound is preferably dispersed in the (4-1) polymer.
  • the compounding ratio of the (1) perovskite compound and the (4-1) polymer may be such that the luminescent action of the (1) perovskite compound is exhibited well.
  • the compounding ratio can be appropriately determined according to the types of (1) perovskite compound and (4-1) polymer.
  • the content ratio of (1) perovskite compound to the total mass of the composition is not particularly limited. Since the content ratio can prevent concentration quenching, it is preferably 90% by mass or less, more preferably 40% by mass or less, further preferably 10% by mass or less, and 3% by mass or less. Is particularly preferable.
  • the content ratio is preferably 0.0002% by mass or more, more preferably 0.002% by mass or more, and 0.01% by mass or more, because good quantum yield can be obtained. Is more preferable.
  • the content ratio of (1) perovskite compound to the total mass of the composition is usually 0.0001 to 30 mass%.
  • the content ratio of the (1) perovskite compound to the total mass of the composition is preferably 0.0001 to 10% by mass, more preferably 0.0005 to 10% by mass, and 0.001 to 3% by mass. Is more preferable.
  • the mass ratio of the (1) perovskite compound to the (4-1) polymer may be 0.00001 to 10, It may be 0.0001 to 2, or 0.0005 to 1.
  • a composition in which the range of the compounding ratio of the (1) perovskite compound and the (4-1) polymer is within the above range is preferable in terms of excellent light emission.
  • the total amount of (1) perovskite compound and (4-1) polymer is 90% by mass or more based on the total mass of the composition.
  • the total amount of the (1) perovskite compound and the (4-1) polymer may be 95% by mass or more, or 99% by mass or more, and 100% by mass based on the total mass of the composition. It may be.
  • the composition of the present embodiment may include the same components as the other components described above.
  • the content ratio of the other components is preferably 10% by mass or less, more preferably 5% by mass or less, and further preferably 1% by mass or less based on the total mass of the composition.
  • composition Containing Component (1), Component (2) and Component (10) contains the (1) component, the (2) component, and the (10) component, The said (2) component with respect to B contained in the (1) component is added.
  • the molar ratio of the nitrogen atoms contained is more than 0 and 0.55 or less, and the ratio of the mass of the nitrogen atoms contained in the component (2) to the mass of the component (10) (nitrogen atom / (10) component). Is 0.5 or less, and the composition has a light emitting property.
  • Component A perovskite compound containing A, B, and X as constituent components.
  • A is a component located at each vertex of a hexahedron centered on B in the perovskite type crystal structure, and is a monovalent cation.
  • X represents a component located at each vertex of an octahedron centered on B in the perovskite type crystal structure, and is at least one anion selected from the group consisting of a halide ion and a thiocyanate ion.
  • B is a component located at the center of a hexahedron having A at its apex and an octahedron having X at its apex in the perovskite crystal structure, and is a metal ion.
  • the molar ratio of the nitrogen atom contained in the (2) amine compound group to B contained in the (1) perovskite compound is the same as that of the first composition of the present embodiment. It is similar to the form, and the same range is preferable.
  • the other embodiment includes the component (1), the component (2) and the component (10), and the ratio of the mass of the nitrogen atom contained in the component (2) to the mass of the component (10) (nitrogen atom / ( The component 10) is 0.5 or less.
  • A is a component located at each vertex of a hexahedron centered on B in the perovskite type crystal structure, and is a monovalent cation.
  • X represents a component located at each vertex of an octahedron centered on B in the perovskite type crystal structure, and is at least one anion selected from the group consisting of a halide ion and a thiocyanate ion.
  • B is a component located at the center of a hexahedron having A at its apex and an octahedron having X at its apex in the perovskite crystal structure, and is a metal ion.
  • the description regarding the (1) perovskite compound and the (2) amine compound group is the same as above.
  • the luminescent semiconductor material of the component (10) will be described.
  • (10) component may be described as (10) semiconductor material.
  • Examples of the light emitting semiconductor material contained in the composition of the present embodiment include the following (i) to (vii).
  • (I) Group II-VI compound semiconductor-containing semiconductor material ii) Group II-V compound semiconductor-containing semiconductor material (iii) Group III-V compound semiconductor-containing semiconductor material (iv) Group III-IV Semiconductor Material Containing Compound Semiconductor (v) Semiconductor Material Containing Group III-VI Compound Semiconductor (vi) Semiconductor Material Containing Group IV-VI Compound Semiconductor (vii) Semiconductor Material Containing Transition Metal-p-Block Compound Semiconductor The (1) perovskite compound is not included in the (10) luminescent semiconductor material.
  • the group II-VI compound semiconductor include a compound semiconductor containing a group 2 element and a group 16 element of the periodic table, and a compound semiconductor containing a group 12 element and a group 16 element of the periodic table.
  • a "periodic table” means a long period type periodic table.
  • a compound semiconductor containing a Group 2 element and a Group 16 element is referred to as a “compound semiconductor (i-1)” and a compound semiconductor containing a Group 12 element and a Group 16 element is referred to as a “compound semiconductor (i-1)”. -2) ".
  • examples of binary compound semiconductors include MgS, MgSe, MgTe, CaS, CaSe, CaTe, SrS, SrSe, SrTe, BaS, BaSe, or BaTe.
  • (i-1), (I-1-1) A ternary compound semiconductor containing one group 2 element and two group 16 elements (i-1-2) Two group 2 elements and one group 16 element A ternary compound semiconductor (i-1-3) containing two kinds of elements and a quaternary compound semiconductor containing two kinds of group 16 elements may be used.
  • binary compound semiconductors include ZnS, ZnSe, ZnTe, CdS, CdSe, CdTe, HgS, HgSe, or HgTe.
  • a ternary compound semiconductor containing one group 12 element and two group 16 elements (i-2-2) two group 12 elements and one group 16 element
  • a ternary compound semiconductor (i-2-3) including two kinds may include a quaternary compound semiconductor including two kinds of Group 12 elements and two kinds of Group 16 elements.
  • the group II-VI compound semiconductor may contain an element other than the group 2 element, the group 12 element, and the group 16 element as a doping element.
  • the group II-V compound semiconductor contains a group 12 element and a group 15 element.
  • binary compound semiconductors include, for example, Zn 3 P 2 , Zn 3 As 2 , Cd 3 P 2 , Cd 3 As 2 , Cd 3 N 2 , or Zn 3 N. 2 .
  • (Ii-1) A ternary compound semiconductor containing one group 12 element and two group 15 elements
  • (ii-2) A ternary compound semiconductor containing two group 12 elements and one group 15 element
  • the compound semiconductor (ii-3) of the group may be a quaternary compound semiconductor containing two kinds of Group 12 elements and two kinds of Group 15 elements.
  • the group II-V compound semiconductor may contain an element other than the group 12 element and the group 15 element as a doping element.
  • the Group III-V compound semiconductor contains a Group 13 element and a Group 15 element.
  • binary compound semiconductors include, for example, BP, AlP, AlAs, AlSb, GaN, GaP, GaAs, GaSb, InN, InP, InAs, InSb, AlN, or BN. Can be mentioned.
  • (Iii-1) A ternary compound semiconductor containing one group 13 element and two group 15 elements
  • (iii-2) A ternary compound semiconductor containing two group 13 elements and one group 15 element System compound semiconductor (iii-3)
  • a quaternary compound semiconductor containing two kinds of Group 13 elements and two kinds of Group 15 elements may be used.
  • the group III-V compound semiconductor may contain an element other than the group 13 element and the group 15 element as a doping element.
  • the group III-IV compound semiconductor contains a group 13 element and a group 14 element.
  • examples of binary compound semiconductors include B 4 C 3 , Al 4 C 3 , and Ga 4 C 3 .
  • the compound semiconductor (iv-3) of the system may be a quaternary compound semiconductor containing two kinds of Group 13 elements and two kinds of Group 14 elements.
  • the group III-IV compound semiconductor may contain an element other than the group 13 element and the group 14 element as a doping element.
  • the group III-VI compound semiconductor contains a group 13 element and a group 16 element.
  • binary compound semiconductors include, for example, Al 2 S 3 , Al 2 Se 3 , Al 2 Te 3 , Ga 2 S 3 , Ga 2 Se 3 , Ga 2 Te 3 , GaTe, In 2 S 3 , In 2 Se 3 , In 2 Te 3 , or InTe.
  • (V-1) A ternary compound semiconductor containing one group 13 element and two group 16 elements
  • (v-2) A ternary compound semiconductor containing two group 13 elements and one group 16 element
  • the compound semiconductor (v-3) of the system may be a quaternary compound semiconductor containing two kinds of group 13 elements and two kinds of group 16 elements.
  • the group III-VI compound semiconductor may contain an element other than the group 13 element and the group 16 element as a doping element.
  • the group IV-VI compound semiconductor contains a group 14 element and a group 16 element.
  • binary compound semiconductors include PbS, PbSe, PbTe, SnS, SnSe, or SnTe.
  • (Vi-1) A ternary compound semiconductor containing one group 14 element and two group 16 elements
  • (vi-2) A ternary compound semiconductor containing two group 14 elements and one group 16 element System compound semiconductor
  • (vi-3) A quaternary compound semiconductor containing two kinds of Group 14 elements and two kinds of Group 16 elements may be used.
  • the group IV-VI compound semiconductor may contain an element other than the group 14 element and the group 16 element as a doping element.
  • the transition metal-p-block compound semiconductor contains a transition metal element and a p-block element.
  • the "p-block element” is an element belonging to Groups 13 to 18 of the periodic table.
  • transition metal-p-block compound semiconductors examples include NiS and CrS.
  • transition metal-p-block compound semiconductor a ternary compound semiconductor containing one kind of (vii-1) transition metal element and two kinds of p-block element, and two kinds of (vii-2) transition metal element It may be a ternary compound semiconductor containing one type, one type of p-block element, or a quaternary compound semiconductor containing two types of (vii-3) transition metal elements and two types of p-block element.
  • the transition metal-p-block compound semiconductor may contain a transition metal element and an element other than the p-block element as a doping element.
  • a compound semiconductor containing Cd which is a Group 12 element and a compound semiconductor containing In which is a Group 13 element are preferable. Further, in the present embodiment, among the above compound semiconductors, a compound semiconductor containing Cd and Se and a compound semiconductor containing In and P are preferable.
  • the compound semiconductor containing Cd and Se is preferably a binary compound semiconductor, a ternary compound semiconductor, or a quaternary compound semiconductor.
  • CdSe which is a binary compound semiconductor, is particularly preferable.
  • the compound semiconductor containing In and P is preferably a binary compound semiconductor, a ternary compound semiconductor, or a quaternary compound semiconductor.
  • InP which is a binary compound semiconductor, is particularly preferable.
  • a semiconductor material containing Cd or a semiconductor material containing In is preferable, and CdSe or InP is more preferable.
  • the second aspect of the composition of the present embodiment is that the mass ratio (nitrogen atom / (10) component) of the nitrogen atom contained in the (2) amine compound group and the (10) semiconductor material is 0.5 or less. Is preferably 0.3 or less, more preferably 0.1 or less, further preferably 0.05 or less, further preferably 0.005 or less, and particularly preferably 0.001 or less.
  • An example of the lower limit of the mass ratio (nitrogen atom / (10) component) of the nitrogen atom contained in the amine compound group to the (10) semiconductor material is 0.0000001, and (1) perovskite From the viewpoint of maintaining the light emission characteristics of the compound, 0.000001 is preferable, 0.00001 is more preferable, and 0.0001 is further preferable.
  • the mass ratio of the nitrogen atoms contained in the (2) amine compound group to the (10) semiconductor material is preferably 0.0000001 or more and 0.5 or less, It is more preferably 0.000001 or more and 0.3 or less, further preferably 0.00001 or more and 0.1 or less, further preferably 0.0001 or more and 0.05 or less, and 0.0001 or more and 0. It is more preferably 0.005 or less, and particularly preferably 0.0001 or more and 0.001 or less.
  • the mass ratio of (10) the light-emitting semiconductor material ( ⁇ g) in the composition and (2) the mass ( ⁇ g) of nitrogen atoms contained in the amine compound group can be calculated by the following formula. .
  • Mass of nitrogen atom contained in amine compound group ( ⁇ g) / (10) Mass of light-emitting semiconductor material ( ⁇ g) mass of nitrogen atom in composition ( ⁇ g) / mass of semiconductor material ( ⁇ g)
  • the mass ( ⁇ g) of nitrogen atoms in the composition was calculated by the following method. (2) Mass of nitrogen atom contained in amine compound group per 1 g of composition ( ⁇ g / g) x mass of composition (g)
  • composition of the present embodiment preferably contains (6) modified product group as an optional component.
  • the group of modified products is represented by silazane, silazane modified product, compound represented by the following formula (C1), modified product of compound represented by the following formula (C1), and formula (C2) below.
  • a silazane modified product a compound modified product represented by the following formula (C1), a compound modified product represented by the following formula (C2), and a compound represented by the following formula (A5-51)
  • a modified product of the compound represented by the formula (1), a modified product of the compound represented by the following formula (A5-52), and a modified product of sodium silicate It is preferable that the modified silazane is used.
  • the group (6) of modified products preferably forms a shell structure as a semiconductor material core in which at least a part of the surface is covered with the surface modifier (5). Specifically, it is preferable that (6) the modified body group overlaps with (5) the surface modifier coating the surface of the semiconductor material, and (5) coats the surface of the surface modifier. ) The surface of the semiconductor material which is not coated with the surface modifier may be coated.
  • the (6) group of modified substances that coat the surface of the semiconductor material or the (5) surface modifier can be confirmed by observing the composition using, for example, SEM or TEM. . Further, detailed element distribution can be analyzed by EDX measurement using SEM or TEM.
  • the term “modified” means that a silicon compound having a Si—N bond, a Si—SR bond (R is a hydrogen atom or an organic group) or a Si—OR bond (R is a hydrogen atom or an organic group) is hydrolyzed. Then, a silicon compound having a Si—O—Si bond is produced.
  • the Si-O-Si bond may be formed by an intermolecular condensation reaction or an intramolecular condensation reaction.
  • the “modified form” refers to a compound obtained by modifying a silicon compound having a Si—N bond, a Si—SR bond or a Si—OR bond.
  • Silazane is a compound having a Si-N-Si bond.
  • the silazane may be linear, branched or cyclic.
  • the silazane may be a low molecular weight silazane or a high molecular weight silazane.
  • the polymer silazane may be referred to as polysilazane.
  • low molecular weight means that the number average molecular weight is less than 600.
  • polymer means that the number average molecular weight is 600 or more and 2000 or less.
  • the “number average molecular weight” means a polystyrene conversion value measured by a gel permeation chromatography (GPC) method.
  • the silazane is preferably a low-molecular silazane, for example, a disilazane represented by the following formula (B1).
  • R 14 and R 15 are each independently a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, an alkenyl group having 1 to 20 carbon atoms, or a cycloalkyl having 3 to 20 carbon atoms. Represents a group, an aryl group having 6 to 20 carbon atoms, or an alkylsilyl group having 1 to 20 carbon atoms.
  • R 14 and R 15 may have a substituent such as an amino group.
  • a plurality of R 15's may be the same or different.
  • Examples of the low-molecular silazane represented by the formula (B1) include 1,3-divinyl-1,1,3,3-tetramethyldisilazane, 1,3-diphenyltetramethyldisilazane, and 1,1,1, 3,3,3-hexamethyldisilazane can be mentioned.
  • silazane for example, a low molecular silazane represented by the following formula (B2) is also preferable.
  • a plurality of R 14's may be the same or different.
  • a plurality of R 15's may be the same or different.
  • n 1 represents an integer of 1 or more and 20 or less. n 1 may be an integer of 1 or more and 10 or less, or 1 or 2.
  • Examples of the low-molecular silazane represented by the formula (B2) include octamethylcyclotetrasilazane, 2,2,4,4,6,6-hexamethylcyclotrisilazane, and 2,4,6-trimethyl-2,4. , 6-trivinylcyclotrisilazane.
  • octamethylcyclotetrasilazane and 1,3-diphenyltetramethyldisilazane are preferable, and octamethylcyclotetrasilazane is more preferable.
  • silazane for example, a polymer silazane represented by the following formula (B3) (polysilazane) is preferable.
  • Polysilazane is a polymer compound having a Si—N—Si bond.
  • the constitutional unit of the polysilazane represented by the formula (B3) may be one kind or plural kinds.
  • R 14, and R 15 are the same as R 14, and R 15 in the formula (B1).
  • * represents a bond.
  • R 14 is bonded to the bond of the nitrogen atom at the end of the molecular chain.
  • R 15 is bonded to the bond of the Si atom at the end of the molecular chain.
  • a plurality of R 14's may be the same or different.
  • a plurality of R 15's may be the same or different.
  • M represents an integer of 2 or more and 10000 or less.
  • the polysilazane represented by the formula (B3) may be, for example, perhydropolysilazane in which all of R 14 and R 15 are hydrogen atoms.
  • the polysilazane represented by the formula (B3) may be, for example, an organopolysilazane in which at least one R 15 is a group other than a hydrogen atom.
  • perhydropolysilazane and organopolysilazane may be appropriately selected, or they may be mixed and used.
  • silazane for example, polysilazane having a structure represented by the following formula (B4) is also preferable.
  • the polysilazane may have a ring structure in a part of the molecule, for example, may have the structure represented by the formula (B4).
  • * represents a bond.
  • the bond of the formula (B4) may be bonded to the bond of the polysilazane represented by the formula (B3) or the bond of the constitutional unit of the polysilazane represented by the formula (B3).
  • the bond of the structure represented by the formula (B4) is a bond of the structure represented by another formula (B4). It may be directly connected to the hand.
  • R 14 is bonded to the bond of the non-nitrogen atom.
  • R 15 is bonded to the bond of the non-Si atom.
  • n 2 represents an integer of 1 or more and 10000 or less. n 2 may be an integer of 1 or more and 10 or less, or 1 or 2.
  • a general polysilazane has, for example, a structure having a linear structure and a ring structure such as a 6-membered ring or an 8-membered ring, that is, a structure represented by (B3) or (B4) above.
  • a general polysilazane has a number average molecular weight (Mn) of about 600 to 2000 (in terms of polystyrene), and may be a liquid or solid substance depending on the molecular weight.
  • a commercially available product may be used as the polysilazane.
  • (Manufactured by the company) AZNN-120-20, Durazane (registered trademark) 1500 Slow Cure, Durazane 1500 Rapid Rapid, Durazane 1800, and Durazane 1033 (manufactured by Merck Performance Materials Co., Ltd.).
  • the polysilazane is preferably AZNN-120-20, Durazane 1500 Slow Cure, Durazane 1500 Rapid Cure, and more preferably Durazane 1500 Slow Cure.
  • the ratio of silicon atoms not bonded to nitrogen atoms is preferably 0.1 to 100% with respect to all silicon atoms. Further, the ratio of silicon atoms not bonded to nitrogen atoms is more preferably 10 to 98%, further preferably 30 to 95%.
  • the “ratio of silicon atoms not bonded to nitrogen atoms” is calculated by using the measurement value described later ((Si (mol)) ⁇ (N (mol) in SiN bond)) / Si (mol) ⁇ Required at 100. Considering the reforming reaction, the “ratio of silicon atoms not bonded to nitrogen atoms” means the “ratio of silicon atoms contained in the siloxane bond generated by the modifying treatment”.
  • the ratio of silicon atoms not bonded to nitrogen atoms is preferably 0.1 to 100% with respect to all silicon atoms. Further, the ratio of silicon atoms not bonded to nitrogen atoms is more preferably 10 to 98%, further preferably 30 to 95%.
  • the ratio of silicon atoms not bonded to nitrogen atoms is preferably 0.1 to 99% with respect to all silicon atoms. Further, the proportion of silicon atoms not bonded to nitrogen atoms is more preferably 10 to 97%, further preferably 30 to 95%.
  • the number of Si atoms and the number of SiN bonds in the modified product can be measured by X-ray photoelectron spectroscopy (XPS).
  • the “ratio of silicon atoms not bonded to nitrogen atoms” of the modified product which is obtained by using the measured value by the above-mentioned method, is preferably 0.1 to 99% with respect to all silicon atoms. It is more preferably from 99 to 99%, further preferably from 30 to 95%.
  • the modified product of silazane is not particularly limited, but a modified product of organopolysilazane is preferable from the viewpoint of improving dispersibility and suppressing aggregation.
  • organopolysilazane examples are represented by the formula (B3), and at least one of R 14 and R 15 is an alkyl group having 1 to 20 carbon atoms, an alkenyl group having 1 to 20 carbon atoms, or 3 to It may be a cycloalkyl group having 20 carbon atoms, an aryl group having 6 to 20 carbon atoms, or an organopolysilazane which is an alkylsilyl group having 1 to 20 carbon atoms.
  • the organopolysilazane includes, for example, a structure represented by the formula (B4), at least one bond is bonded to R 14 or R 15, and at least one of R 14 and R 15 is the number of carbon atoms.
  • the organopolysilazane includes an organopolysilazane represented by the formula (B3) and at least one of R 14 and R 15 is a methyl group, or a structure represented by the formula (B4), and at least one bond is R 14 or It is preferably polysilazane which is bonded to R 15 and at least one of R 14 and R 15 is a methyl group.
  • Y 5 represents a single bond, an oxygen atom or a sulfur atom.
  • R 30 and R 31 are each independently a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or 2 carbon atoms. It represents up to 20 unsaturated hydrocarbon groups.
  • R 30 is an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or an unsaturated hydrocarbon group having 2 to 20 carbon atoms.
  • R 31 represents a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or an unsaturated hydrocarbon group having 2 to 20 carbon atoms.
  • R 30 , R 31 and R 32 are each independently a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 30 carbon atoms, or a carbon atom having 3 to 30 carbon atoms. It represents 2 to 20 unsaturated hydrocarbon groups.
  • the hydrogen atoms contained in the alkyl group, cycloalkyl group and unsaturated hydrocarbon group represented by R 30 , R 31 and R 32 are each independently a halogen atom or amino. It may be substituted with a group.
  • halogen atom which may be substituted for the hydrogen atom contained in the alkyl group, cycloalkyl group or unsaturated hydrocarbon group represented by R 30 , R 31 and R 32 include, for example, a fluorine atom, a chlorine atom and a bromine atom. , And iodine atoms are preferable, and fluorine atoms are preferable from the viewpoint of chemical stability.
  • a is an integer of 1 to 3.
  • a plurality of Y 5 s may be the same or different.
  • a plurality of R 30's may be the same or different.
  • a plurality of R 32's may be the same or different.
  • a plurality of R 31's may be the same or different.
  • the alkyl group represented by R 30 and R 31 may be linear or branched.
  • the number of carbon atoms of the alkyl group represented by R 30 is 1 to 20 because reforming proceeds rapidly. preferable.
  • the number of carbon atoms of the alkyl group represented by R 30 is more preferably 1 to 3, and even more preferably 1.
  • the alkyl group represented by R 30 preferably has 5 to 20 carbon atoms, and 8 to 20 carbon atoms. Is more preferable.
  • Y 5 is preferably an oxygen atom because reforming proceeds rapidly.
  • the number of carbon atoms of the alkyl group represented by R 30 and R 32 is preferably 1 to 20 each independently because reforming proceeds rapidly. Further, the number of carbon atoms of the alkyl group represented by R 30 and R 32 is more preferably independently 1 to 3, and further preferably 1.
  • the alkyl group represented by R 31 preferably has 1 to 5 carbon atoms and 1 to 2 carbon atoms. More preferably, it is more preferably 1.
  • alkyl group represented by R 30 , R 31 and R 32 include the alkyl groups exemplified in the groups represented by R 6 to R 9 .
  • the cycloalkyl group represented by R 30 , R 31 and R 32 preferably has 3 to 20 carbon atoms, and more preferably 3 to 11 carbon atoms.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • the cycloalkyl group represented by R 30 , R 31 and R 32 When the hydrogen atoms in the cycloalkyl group represented by R 30 , R 31 and R 32 are each independently substituted with an alkyl group, the cycloalkyl group has 4 or more carbon atoms.
  • the alkyl group in which the hydrogen atom in the cycloalkyl group may be substituted has 1 to 27 carbon atoms.
  • cycloalkyl group represented by R 30 , R 31 and R 32 include the cycloalkyl groups exemplified in the groups represented by R 6 to R 9 .
  • the unsaturated hydrocarbon group represented by R 30 , R 31 and R 32 may be linear, branched, or cyclic.
  • the unsaturated hydrocarbon group represented by R 30 , R 31 and R 32 preferably has 5 to 20 carbon atoms, and more preferably 8 to 20 carbon atoms.
  • the unsaturated hydrocarbon group represented by R 30 , R 31 and R 32 is preferably an alkenyl group, and more preferably an alkenyl group having 8 to 20 carbon atoms.
  • Examples of the alkenyl group represented by R 30 , R 31 and R 32 include linear or branched alkyl groups exemplified in the groups represented by R 6 to R 9 and having one carbon atom
  • An example is one in which a single bond (C—C) is replaced with a double bond (C ⁇ C).
  • the position of the double bond in the alkenyl group is not limited.
  • alkenyl group examples include, for example, ethenyl group, propenyl group, 3-butenyl group, 2-butenyl group, 2-pentenyl group, 2-hexenyl group, 2-nonenyl group, 2-dodecenyl group, 9 An octadecenyl group.
  • R 30 and R 32 are preferably an alkyl group or an unsaturated hydrocarbon group, and more preferably an alkyl group.
  • R 31 is preferably a hydrogen atom, an alkyl group, or an unsaturated hydrocarbon group, and more preferably an alkyl group.
  • the compound represented by the formula (C1) and the compound represented by the formula (C2) are hydrolyzed. It is liable to be modified and a modified product is easily generated. Therefore, the modified body of the compound represented by the formula (C1) and the modified body of the compound represented by the formula (C2) easily cover the surface of the semiconductor material. As a result, it is considered that (1) the perovskite compound is less likely to deteriorate and a composition having high durability can be obtained.
  • Specific examples of the compound represented by the formula (C1) include tetraethoxysilane, tetramethoxysilane, tetrabutoxysilane, tetrapropoxysilane, tetraisopropoxysilane, 3-aminopropyltriethoxysilane, and 3-aminopropyltrisilane.
  • trimethoxyphenylsilane methoxydimethyl (phenyl) silane, dimethoxydiphenylsilane, dimethoxymethylphenylsilane, cyclohexyltrimethoxysilane, dodecyltriethoxysilane, dodecyltrimethoxysilane, decyltrimethoxysilane, hexyltriethoxysilane, hexyl.
  • the compound represented by the formula (C1) may be dodecyltrimethoxysilane or trimethoxyphenylsilane.
  • a C represents a divalent hydrocarbon group
  • Y 15 represents an oxygen atom or a sulfur atom.
  • R 122 and R 123 each independently represent a hydrogen atom, an alkyl group, or a cycloalkyl group.
  • R 124 represents an alkyl group or a cycloalkyl group.
  • R 125 and R 126 each independently represent a hydrogen atom, an alkyl group, an alkoxy group, or a cycloalkyl group.
  • R 122 to R 126 are alkyl groups, they may be linear or branched.
  • the alkyl group has usually 1 to 20 carbon atoms, preferably 5 to 20 carbon atoms, and more preferably 8 to 20 carbon atoms.
  • the cycloalkyl group may have an alkyl group as a substituent.
  • the cycloalkyl group has usually 3 to 30 carbon atoms, preferably 3 to 20 carbon atoms, and more preferably 3 to 11 carbon atoms.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • the hydrogen atoms contained in the alkyl group and cycloalkyl group represented by R 122 to R 126 may be each independently substituted with a halogen atom or an amino group.
  • halogen atom which may be substituted for the hydrogen atom contained in the alkyl group and cycloalkyl group represented by R 122 to R 126 , include a fluorine atom, a chlorine atom, a bromine atom and an iodine atom.
  • a fluorine atom is preferable from the viewpoint of stability.
  • alkyl group of R 122 to R 126 include the alkyl groups exemplified in R 6 to R 9 .
  • cycloalkyl group of R 122 to R 126 include the cycloalkyl group exemplified in R 6 to R 9 .
  • Examples of the alkoxy group of R 125 and R 126 include monovalent groups in which the linear or branched alkyl group exemplified in R 6 to R 9 is bonded to an oxygen atom.
  • R 125 and R 126 are alkoxy groups, a methoxy group, an ethoxy group, a butoxy group and the like can be mentioned, and a methoxy group is preferable.
  • Divalent hydrocarbon group represented by A C may be any groups from the hydrocarbon compound removal of two hydrogen atoms, said hydrocarbon compound may be an aliphatic hydrocarbon, aromatic It may be a hydrocarbon or a saturated aliphatic hydrocarbon.
  • AC is an alkylene group, it may be linear or branched.
  • the alkylene group has usually 1 to 100 carbon atoms, preferably 1 to 20 carbon atoms, and more preferably 1 to 5 carbon atoms.
  • Examples of the compound represented by the formula (A5-51) include trimethoxy [3- (methylamino) propyl] silane, 3-aminopropyltriethoxysilane, 3-aminopropyldimethoxymethylsilane, and 3-aminopropyldiethoxymethylsilane. , 3-aminopropyltrimethoxysilane is preferred.
  • the compound represented by the formula (A5-51) is preferably a compound in which R 122 and R 123 are hydrogen atoms, R 124 is an alkyl group, and R 125 and R 126 are alkoxy groups.
  • R 122 and R 123 are hydrogen atoms
  • R 124 is an alkyl group
  • R 125 and R 126 are alkoxy groups.
  • 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane are more preferable.
  • 3-aminopropyltrimethoxysilane is more preferable.
  • 3-mercaptopropyltrimethoxysilane and 3-mercaptopropyltriethoxysilane are more preferable.
  • the inorganic silicon compound having a siloxane bond may be a modified form of sodium silicate (Na 2 SiO 3 ).
  • Sodium silicate undergoes hydrolysis to be modified by being treated with an acid.
  • the composition of the present embodiment contains component (1), component (2), and at least one component selected from the group consisting of component (3), component (4), and component (4-1), A composition having a luminescent property in which the molar ratio of the nitrogen atom contained in the component (2) to the B contained in the component (1) is more than 0 and 0.55 or less, further comprising the component (6) It is preferable that the composition has a light emitting property.
  • the composition of this embodiment preferably contains (5) a surface modifier as an optional component.
  • the surface modifier is represented by ammonium ion, amine, primary to quaternary ammonium cation, ammonium salt, carboxylic acid, carboxylate ion, carboxylate salt, and formulas (X1) to (X6), respectively. It contains at least one compound or ion selected from the group consisting of compounds and salts of the compounds represented by formulas (X2) to (X4).
  • the surface modifier preferably contains at least one selected from the group consisting of ammonium ions, amines, primary to quaternary ammonium cations, ammonium salts, carboxylic acids, carboxylate ions and carboxylate salts. And at least one selected from the group consisting of carboxylic acids.
  • the component (5) is (2) the amine compound group.
  • only one compound selected from (5) surface modifier may be used, or two or more compounds may be used in combination.
  • the surface modifier has an effect of adsorbing on the surface of the (1) perovskite compound to stably disperse the (1) perovskite compound in the composition when the (1) perovskite compound is manufactured by the manufacturing method described later. It is a compound that has.
  • ammonium salt a salt containing an ion represented by the following formula (A1).
  • R 1 to R 4 represent a hydrogen atom or a monovalent hydrocarbon group.
  • the hydrocarbon group represented by R 1 to R 4 may be a saturated hydrocarbon group or an unsaturated hydrocarbon group.
  • saturated hydrocarbon group include an alkyl group and a cycloalkyl group.
  • the alkyl group represented by R 1 to R 4 may be linear or branched.
  • the alkyl group represented by R 1 to R 4 usually has 1 to 20 carbon atoms, preferably 5 to 20 carbon atoms, and more preferably 8 to 20 carbon atoms.
  • the number of carbon atoms of the cycloalkyl group is usually 3 to 30, preferably 3 to 20, and more preferably 3 to 11.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • the unsaturated hydrocarbon group of R 1 to R 4 may be linear or branched.
  • the unsaturated hydrocarbon group of R 1 to R 4 usually has 2 to 20 carbon atoms, preferably 5 to 20 carbon atoms, and more preferably 8 to 20 carbon atoms.
  • R 1 to R 4 are preferably a hydrogen atom, an alkyl group, or an unsaturated hydrocarbon group.
  • the unsaturated hydrocarbon group is preferably an alkenyl group.
  • R 1 to R 4 are preferably alkenyl groups having 8 to 20 carbon atoms.
  • alkyl group of R 1 to R 4 include the alkyl groups exemplified in R 6 to R 9 .
  • cycloalkyl group of R 1 to R 4 include the cycloalkyl groups exemplified in R 6 to R 9 .
  • the alkenyl group for R 1 to R 4 is the linear or branched alkyl group exemplified for R 6 to R 9 and is a single bond (C—C) between carbon atoms.
  • Preferred alkenyl groups for R 1 to R 4 include, for example, ethenyl group, propenyl group, 3-butenyl group, 2-butenyl group, 2-pentenyl group, 2-hexenyl group, 2-nonenyl group, 2-dodecenyl group. Group, a 9-octadecenyl group.
  • the counter anion is not particularly limited.
  • the counter anion halide ion, carboxylate ion and the like are preferable.
  • the halide ion include bromide ion, chloride ion, iodide ion, and fluoride ion.
  • ammonium salt having the ammonium cation represented by the formula (A1) and the counter anion include n-octyl ammonium salt and oleyl ammonium salt.
  • the amine as the surface modifier can be represented by the following formula (A11).
  • R 1 ⁇ R 3 represent the same groups as R 1 ⁇ R 3 to the formula (A1) has. However, at least one of R 1 to R 3 is a monovalent hydrocarbon group.
  • the amine as the surface modifier may be any of primary to tertiary amines, but primary amines and secondary amines are preferable, and primary amines are more preferable.
  • Oleylamine is preferred as the amine as the surface modifier.
  • the carboxylate ion, which is a surface modifier is represented by the following formula (A2).
  • the carboxylate salt, which is a surface modifier is a salt containing an ion represented by the following formula (A2). R 5 -CO 2 - ⁇ (A2 )
  • Examples of the carboxylic acid that is the surface modifier include a carboxylic acid having a proton (H + ) bonded to the carboxylate anion represented by (A2) above.
  • R 5 represents a monovalent hydrocarbon group.
  • the hydrocarbon group represented by R 5 may be either a saturated hydrocarbon group or an unsaturated hydrocarbon group.
  • Examples of the saturated hydrocarbon group include an alkyl group and a cycloalkyl group.
  • the alkyl group represented by R 5 may be linear or branched.
  • the alkyl group represented by R 5 usually has 1 to 20 carbon atoms, preferably 5 to 20 carbon atoms, and more preferably 8 to 20 carbon atoms.
  • the number of carbon atoms of the cycloalkyl group is usually 3 to 30, preferably 3 to 20, and more preferably 3 to 11.
  • the number of carbon atoms also includes the number of carbon atoms of the substituent.
  • the unsaturated hydrocarbon group represented by R 5 may be linear or branched.
  • the unsaturated hydrocarbon group represented by R 5 usually has 2 to 20 carbon atoms, preferably 5 to 20 carbon atoms, and more preferably 8 to 20 carbon atoms.
  • R 5 is preferably an alkyl group or an unsaturated hydrocarbon group.
  • the unsaturated hydrocarbon group is preferably an alkenyl group.
  • alkyl group of R 5 include the alkyl groups exemplified in R 6 to R 9 .
  • cycloalkyl group for R 5 include the cycloalkyl groups exemplified for R 6 to R 9 .
  • alkenyl group for R 5 include the alkenyl groups exemplified for R 1 to R 4 .
  • the oleate anion is preferable as the carboxylate anion represented by the formula (A2).
  • the counter cation is not particularly limited, but preferable examples include an alkali metal cation, an alkaline earth metal cation, and an ammonium cation.
  • Oleic acid is preferred as the carboxylic acid that is the surface modifier.
  • R 18 to R 21 each independently have an alkyl group having 1 to 20 carbon atoms, which may have a substituent, or a substituent.
  • the alkyl group represented by R 18 to R 21 may be linear or branched.
  • the alkyl group represented by R 18 to R 21 preferably has an aryl group as a substituent.
  • the alkyl group represented by R 18 to R 21 usually has 1 to 20 carbon atoms, preferably 5 to 20 carbon atoms, and more preferably 8 to 20 carbon atoms.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • the cycloalkyl group represented by R 18 to R 21 preferably has an aryl group as a substituent.
  • the cycloalkyl group represented by R 18 to R 21 usually has 3 to 30 carbon atoms, preferably 3 to 20 carbon atoms, and more preferably 3 to 11 carbon atoms.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • the aryl group represented by R 18 to R 21 preferably has an alkyl group as a substituent.
  • the aryl group represented by R 18 to R 21 usually has 6 to 30 carbon atoms, preferably 6 to 20 carbon atoms, and more preferably 6 to 10 carbon atoms.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • the group represented by R 18 to R 21 is preferably an alkyl group.
  • alkyl group represented by R 18 to R 21 include the alkyl groups exemplified in the alkyl group represented by R 6 to R 9 .
  • cycloalkyl group represented by R 18 to R 21 include the cycloalkyl groups exemplified in the cycloalkyl group represented by R 6 to R 9 .
  • aryl group represented by R 18 to R 21 examples include a phenyl group, a benzyl group, a tolyl group, an o-xylyl group and the like.
  • the hydrogen atoms contained in the groups represented by R 18 to R 21 may each independently be substituted with a halogen atom.
  • the halogen atom include a fluorine atom, a chlorine atom, a bromine atom and an iodine atom.
  • a fluorine atom is preferable as the halogen atom to be substituted because the chemical stability of the compound substituted with a halogen atom is high.
  • M ⁇ represents a counter anion.
  • halide ion As the counter anion, halide ion, carboxylate ion and the like are preferable.
  • the halide ion include bromide ion, chloride ion, iodide ion, and fluoride ion, and bromide ion is preferable.
  • Specific examples of the compound represented by the formula (X1) include tetraethylphosphonium chloride, tetraethylphosphonium bromide, tetraethylphosphonium iodide; tetrabutylphosphonium chloride, tetrabutylphosphonium bromide, tetrabutylphosphonium iodide: tetraphenylphosphonium chloride, tetra Phenylphosphonium bromide, tetraphenylphosphonium iodide; tetra-n-octylphosphonium chloride, tetra-n-octylphosphonium bromide, tetra-n-octylphosphonium iodide; tributyl-n-octylphosphonium bromide; tributyldodecylphosphonium bromide; tributylhexa Decylphospho
  • tributylhexadecylphosphonium bromide and tributyl-n-octylphosphonium bromide are preferable as the compound represented by the formula (X1), and tributyl-n-octylphosphonium. Bromide is more preferred.
  • a 1 represents a single bond or an oxygen atom.
  • R 22 is an alkyl group having 1 to 20 carbon atoms which may have a substituent, and an alkyl group having 3 to 30 carbon atoms which may have a substituent. It represents a cycloalkyl group or an aryl group having 6 to 30 carbon atoms which may have a substituent.
  • the alkyl group represented by R 22 may be linear or branched.
  • alkyl group represented by R 22 the same group as the alkyl group represented by R 18 to R 21 can be adopted.
  • cycloalkyl group represented by R 22 the same group as the cycloalkyl group represented by R 18 to R 21 can be adopted.
  • aryl group represented by R 22 the same group as the aryl group represented by R 18 to R 21 can be adopted.
  • the group represented by R 22 is preferably an alkyl group.
  • the hydrogen atoms contained in the group represented by R 22 may be each independently substituted with a halogen atom, and examples of the halogen atom include a fluorine atom, a chlorine atom, a bromine atom and an iodine atom, From the viewpoint of chemical stability, a fluorine atom is preferable.
  • the anionic group is represented by the following formula (X2-1).
  • an example of the counter cation forming a pair with the formula (X2-1) is an ammonium ion.
  • the counter cation forming a pair in the formula (X2-1) is not particularly limited, but for example, a monovalent ion such as Na + , K + and Cs + can be used. Can be mentioned.
  • the compound represented by the formula (X2) and the salt of the compound represented by the formula (X2) include phenyl phosphate, phenyl disodium phosphate hydrate, 1-naphthyl disodium phosphate hydrate, and 1 -Naphthyl phosphate monosodium monohydrate, lauryl phosphate, sodium lauryl phosphate, oleyl phosphate, benzhydrylphosphonic acid, decylphosphonic acid, dodecylphosphonic acid, ethylphosphonic acid, hexadecylphosphonic acid, heptylphosphonic acid, Hexylphosphonic acid, methylphosphonic acid, nonylphosphonic acid, octadecylphosphonic acid, n-octylphosphonic acid, benzenephosphonic acid, phenylphosphonic acid disodium hydrate, phenethylphosphonic acid, propylphosphonic acid, undecylphosphonic acid,
  • examples of the compound represented by the formula (X2) include oleylphosphoric acid, dodecylphosphonic acid, ethylphosphonic acid, hexadecylphosphonic acid, heptylphosphonic acid, and hexyl.
  • Phosphonic acid, methylphosphonic acid, nonylphosphonic acid, octadecylphosphonic acid and n-octylphosphonic acid are more preferable, and octadecylphosphonic acid is still more preferable.
  • a 2 and A 3 each independently represent a single bond or an oxygen atom.
  • R 23 and R 24 are each independently an alkyl group having 1 to 20 carbon atoms which may have a substituent, or a carbon which may have a substituent. It represents a cycloalkyl group having 3 to 30 atoms or an aryl group having 6 to 30 carbon atoms which may have a substituent.
  • the alkyl groups represented by R 23 and R 24 may each independently be linear or branched.
  • alkyl group represented by R 23 and R 24 the same group as the alkyl group represented by R 18 to R 21 can be adopted.
  • cycloalkyl group represented by R 23 and R 24 the same group as the cycloalkyl group represented by R 18 to R 21 can be adopted.
  • aryl group represented by R 23 and R 24 the same group as the aryl group represented by R 18 to R 21 can be adopted.
  • R 23 and R 24 are preferably each independently an alkyl group.
  • the hydrogen atoms contained in the groups represented by R 23 and R 24 may each independently be substituted with a halogen atom, and examples of the halogen atom include a fluorine atom, a chlorine atom, a bromine atom and an iodine atom. Among them, a fluorine atom is preferable from the viewpoint of chemical stability.
  • the anionic group is represented by the following formula (X3-1).
  • an example of the counter cation forming a pair with the formula (X3-1) is an ammonium ion.
  • the counter cation forming a pair in the formula (X3-1) is not particularly limited, but for example, a monovalent ion such as Na + , K + and Cs + can be used. Can be mentioned.
  • Examples of the compound represented by the formula (X3) include diphenylphosphinic acid, dibutyl phosphate, didecyl phosphate and diphenyl phosphate.
  • Examples of the salt of the compound represented by the formula (X3) include salts of the above compounds.
  • Diphenylphosphinic acid, dibutyl phosphate, and didecyl phosphate are preferable, and diphenylphosphinic acid and salts thereof are more preferable, because the thermal durability of the perovskite compound can be expected to increase.
  • a 4 represents a single bond or an oxygen atom.
  • the group represented by R 25 is an alkyl group having 1 to 20 carbon atoms which may have a substituent, a carbon atom which may have a substituent. It represents a cycloalkyl group of 3 to 30 or an aryl group of 6 to 30 carbon atoms which may have a substituent.
  • alkyl group represented by R 25 the same group as the alkyl group represented by R 18 to R 21 can be adopted.
  • cycloalkyl group represented by R 25 the same group as the cycloalkyl group represented by R 18 to R 21 can be adopted.
  • aryl group represented by R 25 the same group as the aryl group represented by R 18 to R 21 can be adopted.
  • the group represented by R 25 is preferably an alkyl group.
  • the hydrogen atoms contained in the group represented by R 25 may each independently be substituted with a halogen atom, and examples of the halogen atom include a fluorine atom, a chlorine atom, a bromine atom and an iodine atom, From the viewpoint of chemical stability, a fluorine atom is preferable.
  • Examples of the compound represented by the formula (X4) include 1-octanesulfonic acid, 1-decanesulfonic acid, 1-dodecanesulfonic acid, hexadecylsulfate, laurylsulfate, myristylsulfate, laurethsulfate and dodecylsulfate.
  • the anionic group is represented by the following formula (X4-1).
  • examples of the counter cation forming a pair with the formula (X4-1) include ammonium ion.
  • the counter cation forming a pair in the formula (X4-1) is not particularly limited, but for example, a monovalent ion such as Na + , K + and Cs + can be used. Can be mentioned.
  • Examples of the salt of the compound represented by the formula (X4) include sodium 1-octanesulfonate, sodium 1-decanesulfonate, sodium 1-dodecanesulfonate, sodium hexadecyl sulfate, sodium lauryl sulfate, sodium myristyl sulfate and sodium laureth sulfate. , Sodium dodecyl sulfate.
  • a 5 to A 7 each independently represent a single bond or an oxygen atom.
  • R 26 to R 28 are each independently an alkyl group having 1 to 20 carbon atoms which may have a substituent, or a carbon which may have a substituent.
  • a cycloalkyl group having 3 to 30 atoms, an aryl group having 6 to 30 carbon atoms which may have a substituent, an alkenyl group having 2 to 20 carbon atoms which may have a substituent, or a substituent Represents an alkynyl group having 2 to 20 carbon atoms which may have a group.
  • the alkyl groups represented by R 26 to R 28 may each independently be linear or branched.
  • alkyl group represented by R 26 to R 28 the same group as the alkyl group represented by R 18 to R 21 can be adopted.
  • cycloalkyl group represented by R 26 to R 28 the same group as the cycloalkyl group represented by R 18 to R 21 can be adopted.
  • aryl group represented by R 26 to R 28 the same group as the aryl group represented by R 18 to R 21 can be adopted.
  • the alkenyl groups represented by R 26 to R 28 each independently have an alkyl group or an aryl group as a substituent.
  • the alkenyl group represented by R 26 to R 28 usually has 2 to 20 carbon atoms, preferably 6 to 20 carbon atoms, and more preferably 12 to 18 carbon atoms.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • the alkynyl groups represented by R 26 to R 28 each independently preferably have an alkyl group or an aryl group as a substituent.
  • the alkynyl group represented by R 26 to R 28 usually has 2 to 20 carbon atoms, preferably 6 to 20 carbon atoms, and more preferably 12 to 18 carbon atoms.
  • the number of carbon atoms includes the number of carbon atoms of the substituent.
  • R 26 to R 28 are each independently an alkyl group.
  • alkenyl group represented by R 26 to R 28 examples include a hexenyl group, an octenyl group, a decenyl group, a dodecenyl group, a tetradecenyl group, a hexadecenyl group, an octadecenyl group and an icosenyl group.
  • alkynyl group represented by R 26 to R 28 examples include a hexynyl group, an octynyl group, a decynyl group, a dodecynyl group, a tetradecynyl group, a hexadecynyl group, an octadecynyl group, and an icosinyl group.
  • the hydrogen atoms contained in the groups represented by R 26 to R 28 may be independently substituted with a halogen atom, and examples of the halogen atom include a fluorine atom, a chlorine atom, a bromine atom and an iodine atom. Among them, a fluorine atom is preferable from the viewpoint of chemical stability.
  • Examples of the compound represented by the formula (X5) include trioleyl phosphite, tributyl phosphite, triethyl phosphite, trihexyl phosphite, triisodecyl phosphite, trimethyl phosphite, cyclohexyldiphenylphosphine and di-tert.
  • Trioleyl phosphite, tributylphosphine, trihexylphosphine, and trihexyl phosphite are preferable, and trioleyl phosphite is more preferable, because the thermal durability of the perovskite compound can be expected to increase.
  • a 8 to A 10 each independently represent a single bond or an oxygen atom.
  • R 29 to R 31 are each independently an alkyl group having 1 to 20 carbon atoms which may have a substituent, or a carbon which may have a substituent.
  • a cycloalkyl group having 3 to 30 atoms, an aryl group having 6 to 30 carbon atoms which may have a substituent, an alkenyl group having 2 to 20 carbon atoms which may have a substituent, or a substituent Represents an alkynyl group having 2 to 20 carbon atoms which may have a group.
  • the alkyl groups represented by R 29 to R 31 may each independently be linear or branched.
  • alkyl group represented by R 29 to R 31 the same group as the alkyl group represented by R 18 to R 21 can be adopted.
  • cycloalkyl group represented by R 29 to R 31 the same group as the cycloalkyl group represented by R 18 to R 21 can be adopted.
  • aryl group represented by R 29 to R 31 the same group as the aryl group represented by R 18 to R 21 can be adopted.
  • alkenyl group represented by R 29 to R 31 the same group as the alkenyl group represented by R 26 to R 28 can be adopted.
  • alkynyl group represented by R 29 to R 31 the same group as the alkynyl group represented by R 26 to R 28 can be adopted.
  • R 29 to R 31 are preferably each independently an alkyl group.
  • the hydrogen atoms contained in the groups represented by R 29 to R 31 may be independently substituted with a halogen atom, and examples of the halogen atom include a fluorine atom, a chlorine atom, a bromine atom and an iodine atom. Among them, a fluorine atom is preferable from the viewpoint of chemical stability.
  • Examples of the compound represented by the formula (X6) include tri-n-octylphosphine oxide, tributylphosphine oxide, methyl (diphenyl) phosphine oxide, triphenylphosphine oxide, tri-p-tolylphosphine oxide, cyclohexyldiphenylphosphine oxide and phosphorus.
  • Trimethyl phosphate, tributyl phosphate, triamyl phosphate, tris (2-butoxyethyl) phosphate, triphenyl phosphate, tri-p-cresyl phosphate, tri-m-cresyl phosphate, tri-o-cresyl phosphate Can be mentioned.
  • Tri-n-octylphosphine oxide and tributylphosphine oxide are preferable, and tri-n-octylphosphine oxide is more preferable, because the thermal durability of the perovskite compound can be expected to increase.
  • ammonium salts ammonium ions, primary to quaternary ammonium cations, carboxylate salts and carboxylate ions are preferable.
  • ammonium salts and ammonium ions oleylamine salt and oleylammonium ion are more preferable.
  • carboxylate salts and carboxylate ions oleate and oleate cation are more preferable.
  • the compounding ratio of (1) perovskite compound, (2) amine compound group, dispersion medium, (10) semiconductor material, optional (5) surface modifier, and (6) modifier group is Can be appropriately determined according to the type of each component.
  • the blending ratio of each component of the composition described below is not particularly limited as long as the mass of the nitrogen atom contained in the (2) amine compound group is 7600 mass ppm or less with respect to the total mass of the composition.
  • the mass ratio (nitrogen atom / (10) component) of the nitrogen atom contained in the (2) amine compound group to the (10) semiconductor material is 0.5.
  • the following is not particularly limited.
  • composition containing perovskite compound, (2) amine compound group and dispersion medium (1)
  • An example of the compounding ratio of the composition containing perovskite compound, (2) amine compound group and dispersion medium is described in (1) above.
  • the mass ratio [(1) perovskite compound / (dispersion medium)] of the perovskite compound and the dispersion medium is preferably 0.00001 to 10, more preferably 0.0001 to 2, and further preferably 0.0005 to 1, 0.001 to 0.05 is more preferable, and 0.0012 to 0.005 is most preferable.
  • a composition in which the range of the compounding ratio of the perovskite compound and the dispersion medium is within the above range is preferable because the aggregation of the (1) perovskite compound does not easily occur and the luminescent property is excellently exhibited.
  • the molar ratio [Si / B] between (1) the B component of the perovskite compound and (6) the Si element of the modified body group is 0.001 to 2000. It may be 0.01 to 500.
  • the group (6) of modified products when the group (6) of modified products is the silazane represented by the formula (B1) or (B2) and modified products thereof, it is the component B of the perovskite compound (1).
  • the molar ratio [Si / B] of the metal ion to the Si of the (6) modified body group may be 1 to 1000, 10 to 500, or 20 to 300. .
  • the modified product group is a polysilazane having a structure represented by the formula (B3), (1) a metal ion which is a B component of the perovskite compound, and (6)
  • the molar ratio [Si / B] of the modifier group to the Si element may be 0.001 to 2000, 0.01 to 2000, or 0.1 to 1000. It may be 1 to 500 or 2 to 300.
  • composition in which the range of the compounding ratio of the (1) perovskite compound and the (6) modified body group is within the above range exhibits particularly excellent effect of improving the durability of the (6) modified body group. It is preferable in that
  • the molar ratio [Si / B] between the metal ion, which is the B component of the perovskite compound, and the Si element of the modified product can be determined by the following method.
  • the substance amount (B) (unit: mol) of the metal ion that is the B component of the perovskite compound is measured by inductively coupled plasma mass spectrometry (ICP-MS) to measure the mass of the metal that is the B component, and the measured value is the substance amount. Converted to.
  • ICP-MS inductively coupled plasma mass spectrometry
  • the substance amount (Si) of the Si element of the reformer is calculated from the value obtained by converting the mass of the raw material compound of the reformer used into the substance amount and the Si amount (substance amount) contained in the unit mass of the raw material compound. .
  • the unit mass of the raw material compound is the molecular weight of the raw material compound if the raw material compound is a low molecular compound, and the molecular weight of the repeating unit of the raw material compound if the raw material compound is a high molecular compound.
  • the molar ratio [Si / B] can be calculated from the substance amount (Si) of the Si element and the substance amount (B) of the metal ion that is the B component of the perovskite compound.
  • composition containing (1) perovskite compound, (2) amine compound group and (10) semiconductor material (1) Example of compounding ratio of composition containing (1) perovskite compound, (2) amine compound group and (10) semiconductor material
  • mass ratio of the (1) perovskite compound to the (10) semiconductor material [(1) perovskite compound / (10) semiconductor material]
  • 0.00001 to 10 is preferable, and 0.0001 to 2 is more preferable.
  • 0.0005 to 1 is more preferable, 0.001 to 0.5 is more preferable, and 0.005 to 0.1 is further preferable.
  • a composition in which the range of the compounding ratio of the (1) perovskite compound and the (10) semiconductor material is within the above range is preferable in that the light emitting property is also excellently exhibited.
  • composition containing (1) perovskite compound, (2) amine compound group, dispersion medium and (6) modified body group (1) Perovskite compound, (2) amine compound group, dispersion medium and (6) modified body group
  • the mass ratio of the (1) perovskite compound to the total amount of the dispersion medium and the (6) modified body group is preferably 0.00001 to 10, more preferably 0.0001 to 2, further preferably 0.0005 to 1, further preferably 0.001 to 0.05, and 0.1. Most preferred is 0012 to 0.03.
  • a composition in which the range of the compounding ratio of the (1) perovskite compound and the total amount of the dispersion medium and (6) modified body group is within the above range is (1) the perovskite compound is less likely to aggregate, and emits light. Is also preferable in that it is well exhibited.
  • the mass ratio of the (1) perovskite compound to the total amount of the (10) semiconductor material and (6) modified body group is preferably 0.00001 to 10, more preferably 0.0001 to 2, and further preferably 0.0005 to 1, 0.001-0.5 is more preferable, and 0.005-0.1 is further preferable.
  • a composition having a composition ratio of the perovskite compound (1) and the total amount of the (10) semiconductor material and (6) modified substance group within the above range is less likely to cause aggregation of the (1) perovskite compound. Also, it is preferable in that the light emitting property is also excellently exhibited.
  • the surface modifier when the surface modifier is a primary to quaternary ammonium cation which is a compound represented by C 1 N m H n or an ammonium salt thereof, the surface modifier is (2)
  • the compounding ratio of each component in the composition is determined by considering it as an amine compound group.
  • the mass ratio [(1) perovskite compound / ((dispersion medium)] of the above-mentioned (1) perovskite compound and the total amount of the dispersion medium and (5) surface modifier. + (5) surface modifier)] is preferably 0.00001 to 10, more preferably 0.0001 to 2, further preferably 0.0005 to 1, further preferably 0.001 to 0.05, and 0.1. Most preferred is 0012 to 0.005.
  • composition in which the range of the compounding ratio of the (1) perovskite compound and the total amount of the dispersion medium and the (5) surface modifier is within the above range is (1) the perovskite compound is less likely to aggregate, and emits light. Is also preferable in that it is well exhibited.
  • composition containing (1) perovskite compound, (2) amine compound group, dispersion medium, (6) modified substance group, and (5) surface modifier (1) perovskite compound, (2) amine compound group, dispersion medium
  • the mass ratio [(1) perovskite compound / ((dispersion medium) + (6) modifier group + (5) surface modifier)] with respect to the total amount of the surface modifier is preferably 0.00001 to 10, 0.0001 to 2 is more preferable, 0.0005 to 1 is more preferable, 0.001 to 0.05 is further preferable, and 0.0012 to 0.03 is most preferable.
  • composition in which the compounding ratio of the (1) perovskite compound, the dispersion medium, the (6) modified body group, and the total amount of the (5) surface modifier is within the above range is a composition of the (1) perovskite compound. It is preferable because aggregation is unlikely to occur and the light emission property is excellently exhibited.
  • a mass ratio of the (1) perovskite compound to the total amount of the (10) semiconductor material and (5) surface modifier [(1) perovskite compound] / ((10) semiconductor material + (5) surface modifier)] is preferably 0.00001 to 100, more preferably 0.0001 to 20, and more preferably 0.10 from the viewpoint of suppressing deterioration of the (10) semiconductor material.
  • 0005-10 are more preferred, 0.001-5 are more preferred, and 0.005-3 are more preferred.
  • a composition having a composition ratio of the perovskite compound (1) and the total amount of the (10) semiconductor material and (5) surface modifier within the above range is less likely to cause aggregation of the (1) perovskite compound. It is preferable in that the light emitting property is also excellently exhibited.
  • a composition in which the range of the compounding ratio of the (1) perovskite compound to the total amount of the (10) semiconductor material, (6) modified body group, and (5) surface modifier is within the above range is (1) It is preferable in that the perovskite compound is unlikely to aggregate and the luminescence is excellently exhibited.
  • the content ratio of (1) perovskite compound to the total mass of the composition is not particularly limited.
  • the content ratio of the (1) perovskite compound to the total mass of the composition is usually 0.0001 to 30 mass%.
  • the content ratio of the (1) perovskite compound to the total mass of the composition is preferably 0.0001 to 10% by mass, more preferably 0.0005 to 5% by mass, and 0.001 to 3% by mass. Is more preferable.
  • the composition in which the content ratio of the (1) perovskite compound with respect to the total mass of the composition is within the above range is preferable because aggregation of (1) is less likely to occur and the light-emitting property is exhibited well.
  • the dispersion medium may be (3) a solvent alone, (4) a polymerizable compound alone, or (4-1) a polymer alone.
  • a combination with (4-1) polymer is preferable.
  • the blending amount of the above-mentioned (3) solvent means the total amount when two or more kinds are mixed and used.
  • composition of the embodiment according to the present invention can be manufactured.
  • the composition of the present invention is not limited to the one produced by the method for producing a composition of the following embodiments.
  • the second solvent has a lower solubility for the perovskite compound than the first solvent.
  • the solubility means the solubility at the temperature at which the step of mixing the obtained solution and the second solvent is performed.
  • the first solvent and the second solvent at least two kinds selected from the group of organic solvents mentioned above as (a) to (k) can be mentioned.
  • the above-mentioned (d) alcohol, (e) glycol ether, and (f) amide group are used as the first solvent.
  • the organic solvent which it has and (k) dimethyl sulfoxide can be mentioned.
  • the second solvent may be the above-mentioned (a) ester, (b) ketone, (c) ether, or (g). ) Organic solvents having a nitrile group, (h) organic solvents having a carbonate group, (i) halogenated hydrocarbons, and (j) hydrocarbons.
  • the compound containing the component A, the compound containing the component B, and the compound containing the component X are dissolved in the first solvent to obtain a solution.
  • the “compound including the component A” may include the component X.
  • the “compound including the component B” may include the component X.
  • the solution obtained and the second solvent are mixed.
  • the (I) solution may be added to the second solvent, or the (II) second solvent may be added to the solution. Since the perovskite compound produced by the first production method is easily dispersed in the solution, it is advisable to add the solution (I) to the second solvent.
  • the temperature of the solution and the second solvent there is no particular limitation on the temperature of the solution and the second solvent. Since the obtained perovskite compound is easily precipitated, the temperature is preferably in the range of -20 ° C to 40 ° C, more preferably in the range of -5 ° C to 30 ° C. The temperature of the solution and the temperature of the second solvent may be the same or different.
  • the difference in solubility between the first solvent and the second solvent in the perovskite compound is preferably (100 ⁇ g / solvent 100 g) to (90 g / solvent 100 g), and is (1 mg / solvent 100 g) to (90 g / solvent 100 g). Is more preferable.
  • the first solvent is an organic solvent having an amide group such as N, N-dimethylacetamide or dimethyl sulfoxide
  • the second solvent is a halogenated hydrocarbon or a hydrocarbon.
  • the solubility of the first solvent and the second solvent in the perovskite compound when performing the step of mixing at room temperature (10 ° C to 30 ° C) Is preferred because it is easy to control the difference between (100 ⁇ g / solvent 100 g) to (90 g / solvent 100 g).
  • the solubility of the perovskite compound decreases in the resulting mixed solution, and the perovskite compound precipitates. As a result, a dispersion liquid containing the perovskite compound is obtained.
  • the perovskite compound By performing solid-liquid separation on the obtained dispersion liquid containing the perovskite compound, the perovskite compound can be recovered.
  • the solid-liquid separation method include filtration and concentration by evaporation of the solvent. By performing solid-liquid separation, only the perovskite compound can be recovered.
  • the above-mentioned production method preferably includes the step of adding the above-mentioned surface modifier because the perovskite compound obtained is easily and stably dispersed in the dispersion liquid.
  • the step of adding the surface modifier is preferably performed before the step of mixing the solution and the second solvent.
  • the surface modifier may be added to the first solvent, the solution, or the second solvent. Further, the surface modifier may be added to both the first solvent and the second solvent.
  • the above-mentioned manufacturing method includes a step of removing coarse particles by a method such as centrifugation or filtration after the step of mixing the solution and the second solvent.
  • the size of the coarse particles removed in the removing step is preferably 10 ⁇ m or more, more preferably 1 ⁇ m or more, and further preferably 500 nm or more.
  • (Second manufacturing method) As a method for producing a perovskite compound, a step of dissolving a compound including an A component, a compound including a B component, and a compound including an X component, which form the perovskite compound, in a high temperature third solvent, and cooling the solution. And a manufacturing method including a step.
  • the compound containing the component A, the compound containing the component B, and the compound containing the component X are dissolved in a high-temperature third solvent to obtain a solution.
  • the “compound including the component A” may include the component X.
  • the “compound including the component B” may include the component X.
  • each compound may be added to and dissolved in a high temperature third solvent to obtain a solution. Further, in this step, after adding each compound to the third solvent, the temperature may be raised to obtain a solution.
  • the third solvent includes a solvent capable of dissolving a compound containing the component A, which is a raw material, a compound containing the component B, and a compound containing the component X.
  • examples of the third solvent include the above-mentioned first solvent and second solvent.
  • High temperature means the temperature at which each raw material melts.
  • the temperature of the high temperature third solvent is preferably 60 to 600 ° C., and more preferably 80 to 400 ° C.
  • the resulting solution is then cooled.
  • the cooling temperature is preferably ⁇ 20 to 50 ° C., more preferably ⁇ 10 to 30 ° C.
  • the cooling rate is preferably 0.1 to 1500 ° C./min, more preferably 10 to 150 ° C./min.
  • the perovskite compound By cooling the hot solution, the perovskite compound can be precipitated due to the difference in solubility due to the temperature difference between the solutions. As a result, a dispersion liquid containing the perovskite compound is obtained.
  • the perovskite compound can be recovered by solid-liquid separation of the obtained dispersion liquid containing the perovskite compound.
  • the solid-liquid separation method include the method described in the first manufacturing method.
  • the above-mentioned production method preferably includes the step of adding the above-mentioned surface modifier because the perovskite compound obtained is easily and stably dispersed in the dispersion liquid.
  • the step of adding the surface modifier is preferably performed before the step of cooling.
  • the surface modifier may be added to the third solvent, or may be added to the solution containing at least one of the compound containing the component A, the compound containing the component B and the compound containing the component X. Good.
  • a step of removing coarse particles by a method such as centrifugation and filtration shown in the first manufacturing method is included.
  • the manufacturing method includes a step of obtaining the second solution, a step of mixing the first solution and the second solution to obtain a mixed solution, and a step of cooling the obtained mixed solution.
  • the compound containing the component A and the compound containing the component B are dissolved in a high temperature fourth solvent to obtain a first solution.
  • the fourth solvent includes a solvent capable of dissolving the compound containing the component A and the compound containing the component B.
  • examples of the fourth solvent include the above-mentioned third solvent.
  • the “high temperature” may be a temperature at which the compound containing the component A and the compound containing the component B are dissolved.
  • the temperature of the high-temperature fourth solvent is preferably 60 to 600 ° C, more preferably 80 to 400 ° C.
  • a compound containing a compound containing the X component is dissolved in a fifth solvent to obtain a second solution.
  • the compound containing the X component may contain the B component.
  • Examples of the fifth solvent include a solvent capable of dissolving the compound containing the component X.
  • examples of the fifth solvent include the above-mentioned third solvent.
  • the first solution and the second solution obtained are mixed to obtain a mixed solution.
  • mixing the first solution and the second solution one may be dropped on the other. Further, it is advisable to mix the first solution and the second solution while stirring.
  • the cooling temperature is preferably ⁇ 20 to 50 ° C., more preferably ⁇ 10 to 30 ° C.
  • the cooling rate is preferably 0.1 to 1500 ° C./min, more preferably 10 to 150 ° C./min.
  • the perovskite compound By cooling the mixed solution, the perovskite compound can be precipitated due to the difference in solubility due to the difference in temperature of the mixed solution. As a result, a dispersion liquid containing the perovskite compound is obtained.
  • the perovskite compound can be recovered by solid-liquid separation of the obtained dispersion liquid containing the perovskite compound.
  • the solid-liquid separation method include the method described in the first manufacturing method.
  • the above-mentioned production method preferably includes the step of adding the above-mentioned surface modifier because the perovskite compound obtained is easily and stably dispersed in the dispersion liquid.
  • the step of adding the surface modifier is preferably performed before the step of cooling.
  • the surface modifier may be added to any of the fourth solvent, the fifth solvent, the first solution, the second solution and the mixed solution.
  • a step of removing coarse particles by a method such as centrifugation and filtration shown in the first manufacturing method is included.
  • the (1) perovskite compound may include the (2) amine compound group as a residue of the raw material used in the manufacturing process of the (1) perovskite compound. (2) From the viewpoint of reducing the content of the amine compound group, it is preferable to select the third manufacturing method.
  • the semiconductor material that is, the above-mentioned semiconductor materials (i) to (vii) is a mixed liquid obtained by mixing a simple substance of the elements constituting the semiconductor material or a compound of the elements constituting the semiconductor material with a fat-soluble solvent. It can be manufactured by a heating method.
  • Examples of the compound containing an element constituting the semiconductor material are not particularly limited, but include oxides, acetates, organometallic compounds, halides, nitrates and the like.
  • the fat-soluble solvent examples include nitrogen-containing compounds having a hydrocarbon group having 4 to 20 carbon atoms and oxygen-containing compounds having a hydrocarbon group having 4 to 20 carbon atoms.
  • hydrocarbon group having 4 to 20 carbon atoms examples include a saturated aliphatic hydrocarbon group, an unsaturated aliphatic hydrocarbon group, an alicyclic hydrocarbon group, and an aromatic hydrocarbon group.
  • saturated aliphatic hydrocarbon group having 4 to 20 carbon atoms examples include n-butyl group, isobutyl group, n-pentyl group, octyl group, decyl group, dodecyl group, hexadecyl group and octadecyl group.
  • an oleyl group As an unsaturated aliphatic hydrocarbon group having 4 to 20 carbon atoms, an oleyl group can be mentioned.
  • Examples of the alicyclic hydrocarbon group having 4 to 20 carbon atoms include cyclopentyl group and cyclohexyl group.
  • aromatic hydrocarbon group having 4 to 20 carbon atoms examples include phenyl group, benzyl group, naphthyl group and naphthylmethyl group.
  • hydrocarbon group having 4 to 20 carbon atoms a saturated aliphatic hydrocarbon group and an unsaturated aliphatic hydrocarbon group are preferable.
  • Examples of the nitrogen-containing compound include amines and amides.
  • Examples of the oxygen-containing compound include fatty acids.
  • nitrogen-containing compounds having a hydrocarbon group with 4 to 20 carbon atoms are preferable.
  • nitrogen-containing compounds include alkylamines such as n-butylamine, isobutylamine, n-pentylamine, n-hexylamine, octylamine, decylamine, dodecylamine, hexadecylamine and octadecylamine, and oleylamine.
  • Alkenylamines are preferred.
  • a fat-soluble solvent can bind to the surface of a semiconductor material produced by synthesis.
  • Examples of the bond when the lipophilic solvent bonds to the surface of the semiconductor material include chemical bonds such as covalent bond, ionic bond, coordination bond, hydrogen bond, and van der Waals bond.
  • the heating temperature of the above mixed solution may be appropriately set depending on the type of raw material (single substance or compound) used.
  • the heating temperature of the mixed solution is, for example, preferably 130 to 300 ° C, more preferably 240 to 300 ° C. It is preferable for the heating temperature to be at least the above lower limit value because the crystal structure is easily unified. When the heating temperature is not higher than the above upper limit, the crystal structure of the semiconductor material that is produced is less likely to collapse, and the target product is easily obtained, which is preferable.
  • the heating time of the mixed solution may be appropriately set depending on the types of raw materials (single or compound) used and the heating temperature.
  • the heating time of the mixed liquid is, for example, preferably several seconds to several hours, more preferably 1 to 60 minutes.
  • a precipitate containing the target semiconductor material can be obtained.
  • the target semiconductor material can be obtained.
  • a solvent in which the synthesized semiconductor material is insoluble or sparingly soluble is added to reduce the solubility of the semiconductor material in the supernatant liquid to form a precipitate, and the semiconductor material contained in the supernatant liquid is added. You may collect it.
  • the “solvent in which the semiconductor material is insoluble or sparingly soluble” include methanol, ethanol, acetone, acetonitrile and the like.
  • the separated precipitate may be put in an organic solvent (eg, chloroform, toluene, hexane, n-butanol, etc.) to form a solution containing the semiconductor material.
  • an organic solvent eg, chloroform, toluene, hexane, n-butanol, etc.
  • composition obtained by the method 1 for producing a composition is referred to as a “liquid composition”.
  • the liquid composition of the present embodiment can be produced by a production method including a step of mixing (1) a perovskite compound and (3) a solvent and / or (4) one or both of a polymerizable compound.
  • the mixing temperature is preferably 0 ° C to 100 ° C, more preferably 10 ° C to 80 ° C.
  • the (1) perovskite compound may include the (2) amine compound group as a residue of the raw material used in the manufacturing process of the (1) perovskite compound.
  • the production method 1 of the composition may have a step of reducing (2) the content of the amine compound group in advance for the (1) perovskite compound to be used.
  • (1) washing of the perovskite compound can be mentioned.
  • the perovskite compound is preferably washed with the organic solvent described above as (a) to (e) and (h) to (k), using (a) ester and (i) hydrocarbon. It is more preferable to carry out.
  • the surface modifier added as an optional component may behave as (2) the amine compound group.
  • each production method described below includes a step of adjusting the concentration of the (2) amine compound group contained in the obtained composition in order to adjust the concentration of the (2) amine compound group in the obtained composition. But it's okay.
  • a specific method of the step (2) of adjusting the concentration of the amine compound group a method of diluting the obtained composition with a dispersion medium can be mentioned.
  • the method for producing the composition may be the following production method (a1) or production method (a2).
  • Production method (a1) A method for producing a composition comprising: (1) a step of mixing a perovskite compound with (3) a solvent; and (5) a step of mixing the obtained mixture with a surface modifier.
  • Production method (a2) A method for producing a composition comprising the steps of: (1) mixing a perovskite compound with (5) a surface modifier; and mixing the obtained mixture with (3) a solvent.
  • the solvent (3) used in the production methods (a1) and (a2) is preferably one that is difficult to dissolve the above-mentioned (1) perovskite compound.
  • a solvent (3) is preferably one that is difficult to dissolve the above-mentioned (1) perovskite compound.
  • the mixture obtained by the production method (a1) and the composition obtained by the production methods (a1) and (a2) become a dispersion liquid.
  • the method for producing the composition may be the method (a3) using the component (6A) or the method (a4). May be.
  • the component (6A) is referred to as “(6A) raw material compound”.
  • the raw material compound (6A) becomes a group (6) of modified products by subjecting it to a modification treatment.
  • Production method (a3) (1) a step of mixing a perovskite compound and (3) a solvent, a step of mixing the obtained mixture, (5) a surface modifier and (6A) a raw material compound, and the obtained mixture And a step of subjecting the composition to a modification treatment, to produce a composition.
  • the polymer (4-1) may be dissolved or dispersed in the solvent (3).
  • stirring is preferable from the viewpoint of improving dispersibility.
  • the temperature is not particularly limited, but from the viewpoint of uniform mixing, it is preferably in the range of 0 ° C or higher and 100 ° C or lower, and in the range of 10 ° C or higher and 80 ° C or lower. Is more preferable.
  • the production method of the composition is preferably (1) the production method (a1) or the production method (a3) from the viewpoint of improving the dispersibility of the perovskite compound.
  • Modification treatment Method of applying modification treatment
  • examples of the modification treatment method include known methods such as irradiating the (6A) raw material compound with ultraviolet rays, and (6A) reacting the raw material compound with water vapor.
  • the treatment (6A) of reacting the raw material compound with water vapor may be referred to as “humidification treatment”.
  • the wavelength of ultraviolet rays used in the method of irradiating ultraviolet rays is usually 10 to 400 nm, preferably 10 to 350 nm, more preferably 100 to 180 nm.
  • Examples of the light source for generating ultraviolet rays include metal halide lamps, high pressure mercury lamps, low pressure mercury lamps, xenon arc lamps, carbon arc lamps, excimer lamps, and UV laser light.
  • the composition When the humidification treatment is performed, the composition may be left standing or stirred for a certain period of time under the temperature and humidity conditions described below.
  • the temperature in the humidification treatment may be a temperature at which reforming progresses sufficiently.
  • the temperature in the humidifying treatment is, for example, preferably 5 to 150 ° C., more preferably 10 to 100 ° C., and further preferably 15 to 80 ° C.
  • the humidity in the humidification treatment may be such that the water content is sufficiently supplied to the raw material compound (6A) in the composition.
  • the humidity in the humidifying treatment is, for example, preferably 30% to 100%, more preferably 40% to 95%, and further preferably 60% to 90%.
  • the humidity means relative humidity at the temperature at which the humidifying process is performed.
  • the time required for the humidification treatment may be any time that allows the reforming to proceed sufficiently.
  • the time required for the humidifying treatment is, for example, preferably 10 minutes or more and 1 week or less, more preferably 1 hour or more and 5 days or less, and further preferably 2 hours or more and 3 days or less.
  • Stirring is preferable from the viewpoint of enhancing the dispersibility of the raw material compound (6A) contained in the composition.
  • Supply of water in the humidification treatment may be carried out by circulating a gas containing water vapor in the reaction container, or by stirring in an atmosphere containing water vapor, water may be supplied from the interface.
  • the durability of the resulting composition is improved, so that the flow rate of the gas containing water vapor is preferably 0.01 L / min or more and 100 L / min or less, and 0.1 L / min. 10 L / min or less is more preferable, and 0.15 L / min or more and 5 L / min is more preferable.
  • the gas containing steam include nitrogen containing a saturated amount of steam.
  • the surface modifier, (3) solvent, and (6) modified substance group are mixed in any step included in the above-mentioned (1) method for producing a perovskite compound. You may let me.
  • the following manufacturing method (a5) may be used, or the following manufacturing method (a6) may be used.
  • An example of the manufacturing method includes a step of dissolving in a solvent to obtain a solution, and a step of mixing the obtained solution and a second solvent.
  • the first solvent and the second solvent are the same as the above-mentioned solvents.
  • the manufacturing method includes a step of dissolving the solution in a third solvent to obtain a solution, and a step of cooling the solution.
  • the third solvent is the same as the above-mentioned solvent.
  • the conditions of each step included in these production methods are the same as the conditions in the first production method and the second production method in the above-mentioned (1) Production method of perovskite compound.
  • composition of the present embodiment contains (10) semiconductor material
  • “(10) step of mixing semiconductor material” may be appropriately set in the above manufacturing methods (a1) to (a4).
  • the step of (10) mixing the semiconductor material may be set.
  • Production method (c1) (4) a step of dispersing (1) a perovskite compound in a polymerizable compound to obtain a dispersion, the obtained dispersion, (5) a surface modifier, and (6) a group of modified products. And a mixing step.
  • Production method (c2) a step of dispersing (5) a surface modifier and (6) a group of modifiers in (4) a polymerizable compound to obtain a dispersion, the obtained dispersion and (1) a perovskite compound. And a step of mixing.
  • Production method (c3) A production method including a step of dispersing a mixture of (1) a perovskite compound, (5) a surface modifier and (6) a group of modifiers in a polymerizable compound.
  • the production method (c1) is preferable from the viewpoint of (1) enhancing the dispersibility of the perovskite compound.
  • the polymerizable compound (4) in the step of obtaining each dispersion, may be added dropwise to each material, or each material may be added dropwise to the polymerizable compound (4).
  • the polymerizable compound (4) may be added dropwise to each material, or each material may be added dropwise to the polymerizable compound (4).
  • At least one of (1) perovskite compound, (5) surface modifier, and (6) modified body group is preferably added dropwise to (4) polymerizable compound because it is easily dispersed uniformly.
  • the dispersion in each mixing step, may be dropped onto each material, or each material may be dropped onto the dispersion.
  • At least one of the (1) perovskite compound, the (5) surface modifier, and the (6) modified body group is preferably added dropwise to the dispersion because it is easily dispersed uniformly.
  • At least one of the solvent (3) and the polymer (4-1) may be dissolved or dispersed in the polymerizable compound (4).
  • the solvent that dissolves or disperses the polymer is not particularly limited.
  • As the solvent those which are difficult to dissolve the (1) perovskite compound are preferable.
  • Examples of the solvent in which the polymer is dissolved include the same solvents as the above-mentioned first to third solvents.
  • the second solvent is preferred because it has low polarity and is considered to be difficult to dissolve the (1) perovskite compound.
  • hydrocarbon is more preferable.
  • the method for producing the composition of the present embodiment may be the following production method (c4) or production method (c5).
  • Production method (c4) (1) a step of dispersing a perovskite compound in a solvent (3) to obtain a dispersion, and a step of mixing the obtained dispersion with a polymerizable compound (4) to obtain a mixed solution,
  • the manufacturing method of the composition which has the process of mixing the obtained mixed liquid, (5) surface modifier, and (6) modifier group.
  • the method for producing a composition comprising:
  • composition of this embodiment contains (10) a semiconductor material
  • “(10) a step of mixing semiconductor materials” may be appropriately set in the above-described manufacturing methods (c1) to (c5).
  • the step (10) of mixing semiconductor materials may be set after the step of mixing.
  • composition of the present embodiment can be manufactured by a manufacturing method including (1) a step of mixing a perovskite compound and (4) a polymerizable compound, and (4) a step of polymerizing the polymerizable compound.
  • the method of producing the composition of the present embodiment includes a step of mixing (1) a perovskite compound, (5) a surface modifier, (4) a polymerizable compound, and (6) a group of modified substances. And (4) the step of polymerizing the polymerizable compound, can be mentioned.
  • the total of (1) perovskite compound, (5) surface modifier, (4-1) polymer, and (6) modified body group is the total mass of the composition. It is preferably 90% by mass or more.
  • a method for producing the composition of the present embodiment (1) a perovskite compound, (5) a surface modifier, (3) a polymer (4-1) dissolved in a solvent, and (6) A manufacturing method including a step of mixing the modified body group and a step of (3) removing the solvent can also be mentioned.
  • the same mixing method as the method shown in the above-mentioned production method 1 of the composition can be used.
  • Examples of the method for producing the composition include the following production methods (d1) to (d6).
  • Production method (d1) (4) a step of dispersing a (1) perovskite compound in a polymerizable compound to obtain a dispersion, the obtained dispersion, (5) a surface modifier, and (6) a group of modified products.
  • a production method comprising a step of mixing and a step (4) of polymerizing a polymerizable compound.
  • Production method (d3) a step of dispersing (5) a surface modifier and (6) a group of modifiers in a polymerizable compound (4) to obtain a dispersion, the obtained dispersion and (1) a perovskite compound. And a step of polymerizing the polymerizable compound (4).
  • Production method (d4) a step of dispersing (5) a surface modifier and (6) a group of modifiers in (3) a solvent in which (4-1) a polymer is dissolved to obtain a dispersion,
  • a production method comprising a step of mixing a dispersion and (1) a perovskite compound, and a step of removing a solvent.
  • Production method (d5) a step of dispersing a mixture of (1) perovskite compound, (5) surface modifier and (6) modified body group in (4) polymerizable compound, and (4) polymerizable compound And a step of polymerizing the method.
  • Production method (d6) a step of dispersing a mixture of (1) perovskite compound, (5) surface modifier and (6) modified body group in (3) solvent in which (4-1) polymer is dissolved And a step of removing the solvent.
  • the solvent (3) can be removed by, for example, drying at 0 ° C. or higher and 300 ° C. or lower for 1 minute or more and 7 days or less.
  • the step (4) of polymerizing the polymerizable compound included in the production methods (d1), (d3) and (d5) can be carried out by appropriately using a known polymerization reaction such as radical polymerization.
  • radical polymerization a radical polymerization initiator is added to a mixture of (1) perovskite compound, (5) surface modifier, (4) polymerizable compound, and (6) modified body group,
  • the polymerization reaction can be promoted by generating radicals.
  • the radical polymerization initiator is not particularly limited, and examples thereof include a photo radical polymerization initiator.
  • photo-radical polymerization initiator examples include bis (2,4,6-trimethylbenzoyl) -phenylphosphine oxide.
  • composition of the present embodiment contains (10) semiconductor material
  • “(10) step of mixing semiconductor material” may be appropriately set in the above-mentioned manufacturing methods (d1) to (d6).
  • the step of mixing the semiconductor materials may be set.
  • composition Manufacturing Method 3 As the method for producing the composition of the present embodiment, the following production methods (d7) to (d11) can also be adopted.
  • Manufacturing method (d7) a manufacturing method including a step of melt-kneading (1) perovskite compound, (5) surface modifier, and (4-1) polymer.
  • Production method (d9) a step of producing a liquid composition containing (1) a perovskite compound and (5) a surface modifier, a step of extracting a solid content from the obtained liquid composition, and a obtained solid content And a step of melt-kneading (4-1) the polymer.
  • Production method (d10) (1) a step of producing a liquid composition containing a perovskite compound, (5) a surface modifier, and (6) a group of modifiers, and taking out a solid content from the obtained liquid composition.
  • a production method comprising the steps of: and a step of melt-kneading the obtained solid content and (4-1) polymer.
  • a mixture of the (4-1) polymer and another material may be melt-kneaded, and the melted (4-1) polymer may be mixed with other materials. Materials may be added.
  • the "other material” refers to a material used in each production method in addition to the (4-1) polymer, specifically, (1) perovskite compound, (5) surface modifier, (6A) raw material compound and (6) Refers to a modified body group.
  • the (6) modified body group added in the melt-kneading step of the production method (d11) is obtained by modifying the raw material compound (6A).
  • melt-kneading the polymer (4-1) in the production methods (d7) to (d11) a known method of kneading the polymer can be adopted.
  • extrusion processing using a single screw extruder or a twin screw extruder can be adopted.
  • the method described above can be adopted for the step of performing the modification treatment of the manufacturing method (d8).
  • the above-mentioned production method (a1) or (a2) can be adopted in the step of producing the liquid composition of the production methods (d9) and (d11).
  • the above-mentioned production method (a3) or (a4) can be adopted in the step of producing the liquid composition of the production method (d10).
  • composition of the present embodiment contains (10) semiconductor material
  • “(10) step of mixing semiconductor material” may be appropriately set in the above manufacturing methods (d7) to (d11).
  • the step of producing the liquid composition may include the step of mixing (10) the semiconductor material, and (1) together with the (10) semiconductor material and (4-) 1) The polymer may be melt-kneaded.
  • the amount of the luminescent semiconductor material contained in the composition of the present invention is calculated as the solid content concentration (mass%) by the dry mass method.
  • the emission intensity is measured using an absolute PL quantum yield measuring device (C9920-02, manufactured by Hamamatsu Photonics KK) under excitation light of 450 nm, room temperature, and the atmosphere.
  • the film according to this embodiment uses the above-mentioned composition as a forming material.
  • the film according to the present embodiment contains (1) perovskite compound and (4-1) polymer, and the total of (1) perovskite compound and (4-1) polymer is 90% by mass relative to the total mass of the film. % Or more.
  • the shape of the film is not particularly limited and may be any shape such as a sheet shape or a bar shape.
  • the “bar-like shape” means, for example, a band-like shape in plan view extending in one direction. Examples of the band-like shape in plan view include a plate-like shape in which each side has a different length.
  • the thickness of the film may be 0.01 ⁇ m to 1000 mm, 0.1 ⁇ m to 10 mm, or 1 ⁇ m to 1 mm.
  • the thickness of the film refers to the front surface and the back surface in the thickness direction of the film when the side having the smallest value among the length, width and height of the film is defined as the “thickness direction”. Refers to the distance between. Specifically, the thickness of the film is measured at any three points on the film using a micrometer, and the average value of the measured values at the three points is taken as the film thickness.
  • the film may be a single layer or multiple layers. In the case of multiple layers, the same type of composition may be used for each layer, or different types of compositions may be used for each layer.
  • the film can be obtained as a film formed on a substrate, for example, by the laminated structure manufacturing methods (e1) to (e3) described below. Further, the film can be obtained by peeling it from the substrate.
  • the laminated structure according to the present embodiment has a plurality of layers, and at least one layer is the above-mentioned film.
  • examples of layers other than the above-mentioned films include arbitrary layers such as a substrate, a barrier layer, and a light scattering layer.
  • the shape of the laminated film is not particularly limited, and may be any shape such as a sheet shape and a bar shape.
  • the substrate is not particularly limited, but may be a film.
  • the substrate is preferably light transmissive.
  • a laminated structure having a light-transmitting substrate is preferable because it is easy to take out the light emitted by the (1) perovskite compound.
  • a material for forming the substrate for example, a polymer such as polyethylene terephthalate or a known material such as glass can be used.
  • a polymer such as polyethylene terephthalate or a known material such as glass can be used.
  • the above-mentioned film may be provided on the substrate.
  • FIG. 1 is a sectional view schematically showing the configuration of the laminated structure of this embodiment.
  • the film 10 of the present embodiment is provided between the first substrate 20 and the second substrate 21.
  • the film 10 is sealed by the sealing layer 22.
  • One aspect of the present invention is a first substrate 20, a second substrate 21, a film 10 according to the present embodiment located between the first substrate 20 and the second substrate 21, and a sealing.
  • a laminated structure having a layer 22 and the encapsulating layer 22 is disposed on a surface of the film 10 which is not in contact with the first substrate 20 and the second substrate 21. It is the structure 1a.
  • the layer that the laminated structure according to the present embodiment may have is not particularly limited, and examples thereof include a barrier layer.
  • a barrier layer may be included from the viewpoint of protecting the above-mentioned composition from water vapor in the outside air and air in the atmosphere.
  • the barrier layer is not particularly limited, but is preferably transparent from the viewpoint of extracting emitted light.
  • a polymer such as polyethylene terephthalate or a known barrier layer such as a glass film can be used.
  • the layer that the laminated structure according to the present embodiment may have is not particularly limited, and examples thereof include a light scattering layer. From the viewpoint of effectively utilizing the incident light, a light scattering layer may be included.
  • the light scattering layer is not particularly limited, but is preferably transparent from the viewpoint of extracting emitted light.
  • As the light scattering layer light scattering particles such as silica particles, or a known light scattering layer such as an amplification diffusion film can be used.
  • the light emitting device according to this embodiment can be obtained by combining the film or laminated structure of this embodiment with a light source.
  • the light-emitting device is a device that emits light by irradiating a film or a laminated structure provided in a light emission direction of the light source with light emitted from the light source so that the film or the laminated structure emits light.
  • the layers other than the above-mentioned film, substrate, barrier layer, and light scattering layer include a light reflection member, a brightness enhancement portion, a prism sheet, a light guide plate, and a medium between elements Any layer such as a material layer may be used.
  • One aspect of the present invention is a light emitting device 2 in which a prism sheet 50, a light guide plate 60, a first laminated structure 1a, and a light source 30 are laminated in this order.
  • a light source that emits light included in the absorption wavelength band of the (1) perovskite compound is used as a light source forming the light emitting device of the present embodiment.
  • a light source having an emission wavelength of 600 nm or less is preferable.
  • a known light source such as a light emitting diode (LED) such as a blue light emitting diode, a laser, or an EL can be used.
  • the layer that may be included in the laminated structure forming the light emitting device of the present embodiment is not particularly limited, and examples thereof include a light reflecting member.
  • a light emitting device having a light reflecting member can efficiently irradiate light from a light source toward a film or a laminated structure.
  • the light reflection member is not particularly limited, but may be a reflection film.
  • a known reflecting film such as a reflecting mirror, a film of reflecting particles, a reflecting metal film or a reflector can be used.
  • the layer that may be included in the laminated structure that configures the light emitting device of the present embodiment is not particularly limited, and examples thereof include a brightness enhancement portion.
  • the brightness enhancement section may be included from the viewpoint of reflecting a part of the light back toward the direction in which the light is transmitted.
  • the layer that may be included in the laminated structure that configures the light emitting device of the present embodiment is not particularly limited, but a prism sheet can be used.
  • the prism sheet typically has a base material portion and a prism portion. The base material portion may be omitted depending on the adjacent member.
  • the prism sheet can be attached to an adjacent member via any appropriate adhesive layer (eg, adhesive layer, pressure-sensitive adhesive layer).
  • adhesive layer e.g, adhesive layer, pressure-sensitive adhesive layer.
  • the prism sheet is configured by arranging a plurality of unit prisms that are convex on the side opposite to the viewing side (back side).
  • the convex portion of the prism sheet By arranging the convex portion of the prism sheet so as to face the back surface side, it becomes easy to collect light that passes through the prism sheet.
  • the convex portion of the prism sheet is arranged facing the back side, compared to the case where the convex portion is arranged facing the viewing side, less light is reflected without entering the prism sheet, and a display with high brightness is displayed. Can be obtained.
  • the layer that may be included in the laminated structure that configures the light emitting device of the present embodiment is not particularly limited, and examples thereof include a light guide plate.
  • a light guide plate for example, a light guide plate having a lens pattern formed on the back side so that light from the lateral direction can be deflected in the thickness direction, a prism shape on either or both of the back side and the viewing side. Any suitable light guide plate may be used, such as a light guide plate on which the like is formed.
  • the layer that may be included in the laminated structure that constitutes the light emitting device of the present embodiment is not particularly limited, but a layer composed of one or more medium materials (on the optical path between adjacent elements (layers) ( Media material layers between elements).
  • the one or more media contained in the media material layer between the elements include, but are not limited to, vacuum, air, gas, optical material, adhesive, optical adhesive, glass, polymer, solid, liquid, gel, cured. Materials, optical coupling materials, index matching or index mismatching materials, gradient index materials, cladding or anti-cladding materials, spacers, silica gel, brightness enhancing materials, scattering or diffusing materials, reflective or anti-reflective materials, wavelength selection Materials, wavelength selective anti-reflective materials, color filters, or suitable media known in the art.
  • the light emitting device of the present embodiment include those provided with a wavelength conversion material for EL displays and liquid crystal displays. Specifically, the following respective structures (E1) to (E4) can be mentioned.
  • composition of the present embodiment is put in a glass tube or the like and sealed, and the composition is arranged between the blue light emitting diode as a light source and the light guide plate so as to be along the end surface (side surface) of the light guide plate. Then, a backlight that converts blue light into green light or red light (on-edge backlight).
  • the composition of the present embodiment is formed into a sheet, and a film obtained by sandwiching the composition with two barrier films and sealing is placed on the light guide plate and placed on the end surface (side surface) of the light guide plate.
  • a backlight surface-mounted backlight that converts blue light emitted from the blue light emitting diode to the sheet through a light guide plate into green light or red light.
  • E3 A backlight (on-chip) that disperses the composition of the present embodiment in a resin or the like and installs it in the vicinity of a light emitting portion of a blue light emitting diode to convert the emitted blue light into green light or red light. Method backlight).
  • the composition of the present embodiment is molded and placed in the subsequent stage of the blue light emitting diode as a light source to convert blue light into green light or red light. Illumination that emits white light is included.
  • the display 3 of this embodiment includes a liquid crystal panel 40 and the above-described light emitting device 2 in this order from the viewing side.
  • the light emitting device 2 includes a second stacked structure body 1b and a light source 30.
  • the above-mentioned first laminated structure 1a further includes a prism sheet 50 and a light guide plate 60.
  • the display may further comprise any suitable other member.
  • One aspect of the present invention is a liquid crystal display 3 in which a liquid crystal panel 40, a prism sheet 50, a light guide plate 60, a first laminated structure 1a, and a light source 30 are laminated in this order.
  • the liquid crystal panel typically includes a liquid crystal cell, a viewing side polarizing plate arranged on the viewing side of the liquid crystal cell, and a back side polarizing plate arranged on the back side of the liquid crystal cell.
  • the viewing-side polarizing plate and the back-side polarizing plate may be arranged such that their absorption axes are substantially orthogonal or parallel.
  • the liquid crystal cell has a pair of substrates and a liquid crystal layer as a display medium sandwiched between the pair of substrates.
  • one substrate is provided with a color filter and a black matrix
  • the other substrate is provided with a switching element for controlling electro-optical characteristics of liquid crystal and a scanning line for giving a gate signal to this switching element.
  • a signal line for supplying a source signal, a pixel electrode, and a counter electrode.
  • the distance (cell gap) between the substrates can be controlled by a spacer or the like.
  • An alignment film made of polyimide, for example, can be provided on the side of the substrate that is in contact with the liquid crystal layer.
  • the polarizing plate typically has a polarizer and protective layers disposed on both sides of the polarizer.
  • the polarizer is typically an absorption-type polarizer.
  • any suitable polarizer is used as the polarizer.
  • a dichroic substance such as iodine or a dichroic dye is adsorbed on a hydrophilic polymer film such as a polyvinyl alcohol film, a partially formalized polyvinyl alcohol film, or an ethylene / vinyl acetate copolymer partially saponified film.
  • Uniaxially stretched film, polyene oriented film such as polyvinyl alcohol dehydrated product, polyvinyl chloride dehydrochlorinated product and the like.
  • a polarizer obtained by uniaxially stretching a polyvinyl alcohol film by adsorbing a dichroic substance such as iodine has a high polarization dichroic ratio, and is particularly preferable.
  • composition of the present embodiment include the following uses.
  • composition of this embodiment can be used, for example, as a material for a light emitting layer of a light emitting diode (LED).
  • the LED including the composition of the present embodiment for example, the composition of the present embodiment and conductive particles such as ZnS are mixed and laminated in a film shape, the n-type transport layer is laminated on one surface, and the other surface is laminated on the other surface. It has a structure in which p-type transport layers are stacked, and when a current is passed, holes in the p-type semiconductor and electrons in the n-type semiconductor are charged in the composition of the junction surface in (1) the perovskite compound. There is a method of emitting light by canceling.
  • composition of the present embodiment can be used as an electron transporting material contained in the active layer of a solar cell.
  • the structure of the solar cell is not particularly limited, but examples thereof include a fluorine-doped tin oxide (FTO) substrate, a titanium oxide dense layer, a porous aluminum oxide layer, an active layer containing the composition of the present invention, 2, 2
  • FTO fluorine-doped tin oxide
  • TiO titanium oxide dense layer
  • porous aluminum oxide layer an active layer containing the composition of the present invention
  • a hole transport layer such as', 7,7'-tetrakis (N, N'-di-p-methoxyphenylamine) -9,9'-spirobifluorene (Spiro-MeOTAD) and a silver (Ag) electrode are provided in this order.
  • a solar cell is mentioned.
  • the titanium oxide dense layer has a function of electron transport, an effect of suppressing the roughness of FTO, and a function of suppressing reverse electron transfer.
  • the porous aluminum oxide layer has a function of improving light absorption efficiency.
  • composition of the present embodiment contained in the active layer has the functions of charge separation and electron transport.
  • the composition of the present embodiment is applied to a living body such as an image detection unit (image sensor) for a solid-state imaging device such as an X-ray imaging device and a CMOS image sensor, a fingerprint detection unit, a face detection unit, a vein detection unit and an iris detection unit. It can be used as a photoelectric conversion element (photodetection element) material included in a detection section for detecting a predetermined characteristic of a part or a detection section of an optical biosensor such as a pulse oximeter.
  • a photoelectric conversion element photodetection element
  • Examples of the film production method include the following production methods (e1) to (e3).
  • Manufacturing method (e1) A method for manufacturing a film, which includes a step of applying a liquid composition to obtain a coating film, and a step of (3) removing a solvent from the coating film.
  • a method of manufacturing a film including.
  • Production method (e3) A method for producing a film by molding the composition obtained by the above-mentioned production methods (d1) to (d6).
  • the film produced by the above production methods (e1) and (e2) may be peeled off from the production position and used.
  • Examples of the method for manufacturing the laminated structure include the following manufacturing methods (f1) to (f3).
  • Production method (f1) Lamination including a step of producing a liquid composition, a step of applying the obtained liquid composition onto a substrate, and a step of removing (3) a solvent from the obtained coating film Structure manufacturing method.
  • Manufacturing method (f2) A manufacturing method of a laminated structure including a step of attaching a film to a substrate.
  • Production method (f3) (4) A step of producing a liquid composition containing a polymerizable compound, a step of applying the obtained liquid composition on a substrate, and a step of applying the obtained coating film (4) And a step of polymerizing the polymerizable compound.
  • the above-mentioned manufacturing methods (c1) to (c5) can be adopted in the steps of manufacturing the liquid composition in the manufacturing methods (f1) and (f3).
  • the step of applying the liquid composition on the substrate in the production methods (f1) and (f3) is not particularly limited, but is a gravure coating method, a bar coating method, a printing method, a spray method, a spin coating method, a dip method, Known coating and coating methods such as a die coating method can be used.
  • the step of removing the solvent (3) in the production method (f1) may be the same step as the step of removing the solvent (3) included in the production methods (d2), (d4), and (d6) described above. it can.
  • the step of polymerizing the (4) polymerizable compound in the production method (f3) is the same as the step of polymerizing the (4) polymerizable compound contained in the above-mentioned production methods (d1), (d3), and (d5). be able to.
  • any adhesive can be used.
  • the adhesive is not particularly limited as long as it does not dissolve (1) the perovskite compound and (10) the semiconductor material, and a known adhesive can be used.
  • the method for producing a laminated structure may further include a step of laminating an arbitrary film on the obtained laminated structure.
  • a reflection film or a diffusion film can be mentioned.
  • Arbitrary adhesives can be used in the process of laminating the films.
  • the above-mentioned adhesive is not particularly limited as long as it does not dissolve (1) the perovskite compound and (10) the semiconductor material, and known adhesives can be used.
  • ⁇ Manufacturing Method of Light-Emitting Device For example, a manufacturing method including the above-mentioned light source and a step of installing the above-mentioned film or laminated structure on the optical path of light emitted from the light source can be mentioned.
  • the concentration of the (1) perovskite compound in the compositions obtained in Experimental Examples 1 to 4, Examples 1 to 4 and Comparative Examples 1 and 2 was measured by the following method. First, the perovskite compound was dissolved by adding N, N-dimethylformamide to the dispersion liquid containing the perovskite compound and the solvent obtained by redispersion. After that, Pb and Cs were measured with ICP-MS (ELAN DRCII manufactured by PerkinElmer), and Br was measured using an ion chromatograph (Integration manufactured by Thermo Fisher Scientific Co., Ltd.) to calculate the total.
  • ICP-MS ELAN DRCII manufactured by PerkinElmer
  • Quantera SXM manufactured by ULVAC-PHI, Inc. AlK ⁇ ray photoelectron take-off angle of 45 degrees, aperture diameter of 100 ⁇ m, peak attributed to C1s of surface contaminated hydrocarbons was 284.6 eV and used as a standard for charging correction.
  • the mass of nitrogen atom contained in the amine compound group in the composition was calculated by the following formula from the Pb content ( ⁇ g / g) in the perovskite contained in the composition obtained by the above ICP-MS measurement. did.
  • Molar ratio of nitrogen atom contained in amine compound group to Pb contained in perovskite compound mass of amine compound group in composition (GC-MS measurement value, ⁇ g / g) / molecular weight of amine compound group in composition ( g / mol) ⁇ number of nitrogen atoms contained in one molecule of the amine compound group in the composition / Pb ( ⁇ g / g: ICP measurement value) ⁇ Pb (g / mol)
  • the amount of increase in the half width of the peak A of the luminescent semiconductor material in the composition is ⁇ 0.2 or more and 1.03 or less. It is excellent as a luminescent composition.
  • the emission intensity ratio of the peak (peak B) giving the maximum emission intensity of the emission spectrum derived from the perovskite compound immediately after mixing and 1 hour after mixing was calculated by the following formula.
  • (Emission intensity ratio of peak B immediately after mixing and 1 hour after mixing) (Emission intensity of peak B after 1 hour of mixing) / (Emission intensity of peak B immediately after mixing)
  • the emission intensity ratio of peak B immediately after mixing and after 1 hour of mixing is 0.5 or more and 1.0 or less, which indicates the emission intensity when used as a light emitting material From the viewpoint of maintaining, it is excellent as a luminescent composition.
  • 0.276 g of lead bromide (PbBr 2 ) was mixed with 20 mL of 1-octadecene solvent. After stirring with a magnetic stirrer and heating at a temperature of 120 ° C. for 1 hour while flowing nitrogen, 2 mL of oleic acid and 2 mL of oleylamine were added to prepare a lead bromide dispersion liquid. After raising the temperature of the lead bromide dispersion to 160 ° C., 1.6 mL of the above cesium carbonate solution was added. After the addition, the reaction vessel was soaked in ice water to lower the temperature to room temperature to obtain a dispersion liquid.
  • the dispersion was centrifuged at 10,000 rpm for 5 minutes to separate the precipitate, whereby a perovskite compound of the precipitate was obtained.
  • the perovskite compound was dispersed in 5 mL of toluene to obtain a perovskite dispersion liquid 1.
  • the concentration of the perovskite compound measured by ICP-MS and ion chromatography of the obtained perovskite dispersion liquid 1 was 15000 ppm ( ⁇ g / g).
  • the content of nitrogen atoms derived from the amine compound group contained in the above dispersion containing the perovskite was calculated from the nitrogen atoms / Pb measured by XPS and the Pb amount measured by ICP-MS, and was 290 ppm ( ⁇ g / g) there were.
  • the dispersion composition had a content of nitrogen atoms derived from the amine compound group of 207 ppm ( ⁇ g / g), and the mass ratio of the luminescent semiconductor material in the dispersion composition and the nitrogen atom in the amine compound group was 0. It was 0.0145.
  • the value of [(emission intensity derived from semiconductor material after 1 hour) / (emission intensity derived from semiconductor material immediately after mixing semiconductor material)] was 0.36.
  • the emission spectrum was measured by mixing the dispersion composition having a nitrogen atom amount of 207 ppm ( ⁇ g / g) derived from the amine compound group with 2.25 mL of toluene and diluting it, and further collecting 0.01 mL of the dispersion composition. A solution obtained by mixing 2.99 mL of toluene was measured.
  • Example 2 0.25 mL of a 0.25 mL perovskite dispersion 1 obtained by the same method as in Experimental Example 1 and a commercially available toluene dispersion of InP / ZnS (solid content concentration 5% of luminescent semiconductor material: emission wavelength 630 nm) were mixed. Then, a dispersion liquid composition containing InP having a nitrogen atom amount derived from the amine compound group of 145 ppm ( ⁇ g / g) and perovskite was obtained. The mass ratio of the luminescent semiconductor material in the dispersion composition and the nitrogen atom in the amine compound group was 0.0058.
  • the value of [(emission intensity derived from semiconductor material after 1 hour) / (emission intensity derived from semiconductor material immediately after mixing of semiconductor materials)] was 0.40.
  • the emission spectrum was measured by mixing the dispersion composition in which the content of nitrogen atoms derived from the amine compound group was 145 ppm ( ⁇ g / g) with 2.25 mL of toluene and diluting it, and further adding 0.01 mL thereof. A solution obtained by taking 2.99 mL of toluene was measured.
  • Example 3 0.5 mL of 0.25 mL perovskite dispersion 1 obtained by the same method as in Experimental Example 1 and commercially available toluene dispersion of InP / ZnS (solid content concentration of luminescent semiconductor material: 5%: emission wavelength 630 nm) And mixed to obtain a dispersion composition in which the amount of N derived from the amine compound group is 97 ppm ( ⁇ g / g).
  • the mass ratio of the luminescent semiconductor material in the dispersion composition and N in the amine compound group was 0.00290.
  • the mass ratio of the luminescent semiconductor material in the composition to the lead atom in the perovskite measured by ICP-MS was 0.0715.
  • the value of [emission intensity derived from semiconductor material after 1 hour) / (emission intensity derived from semiconductor material immediately after mixing of semiconductor materials)] was 0.49.
  • the value of [(Full width at half maximum of light emission from semiconductor material after 1 hour)-(Full width at half maximum of light emission from semiconductor material immediately after mixing of semiconductor materials)] was 1.04 nm.
  • the value of [(emission intensity of emission from perovskite compound after 1 hour) / (emission intensity from perovskite compound immediately after mixing of semiconductor material)] was 1.0.
  • the emission spectrum was measured by mixing the dispersion composition in which the amount of N derived from the amine compound group was 97 ppm with 2.25 mL of toluene and diluting it, and further collecting 0.01 mL therefrom to obtain 2.99 mL of toluene.
  • the mixed solution was measured.
  • a dispersion liquid composition containing InP and perovskite having a nitrogen atom amount derived from the amine compound group of 1579 ppm ( ⁇ g / g), an amine compound group, and a solvent were obtained.
  • the mass ratio of nitrogen atoms contained in the amine compound group in the composition to the mass ratio of nitrogen atoms in the light emitting semiconductor material (nitrogen atom / (10) component) was 0.11.
  • the value of [(emission intensity derived from semiconductor material after 1 hour) / (emission intensity derived from semiconductor material immediately after mixing of semiconductor materials)] was 0.30.
  • the emission spectrum was measured by mixing the dispersion composition in which the amount of nitrogen atoms derived from the amine compound group was 1579 ppm ( ⁇ g / g) with 2.25 mL of toluene, and then diluting 0.01 mL thereof. A solution obtained by mixing 2.99 mL of toluene was measured.
  • Example 1 The perovskite dispersion liquid 1 obtained in the same manner as in Experimental Example 1 was centrifuged at 10,000 rpm for 5 minutes to separate the precipitate, and then the precipitate was dispersed in a mixed solution of 5 mL of ethyl acetate and 15 mL of toluene, and then 10,000 rpm, The precipitate was washed by centrifugation for 5 minutes. By washing three times, a perovskite compound as a precipitate was obtained and then redispersed in toluene.
  • the concentration of the perovskite compound measured by ICP-MS and ion chromatography was 15000 ppm ( ⁇ g / g). 0.05 ml of the above-mentioned dispersion containing the perovskite was collected.
  • the nitrogen amount derived from the amine compound group and the molar ratio of Pb (N / Pb) contained in the above-described dispersion containing perovskite were 0.3 as measured by XPS.
  • the amount of nitrogen derived from the amine compound group contained in the above-mentioned dispersion containing perovskite was 145 ppm ( ⁇ g / g) calculated from the amount of Nb / Pb measured by XPS and the amount of Pb measured by ICP-MS.
  • 0.1 mL of a commercially available toluene dispersion of InP / ZnS (solid content of luminescent semiconductor material: 5%; emission wavelength: 630 nm) was added to the dispersion composition containing the perovskite, the solvent, and the amine compound group.
  • a dispersion liquid composition containing InP and perovskite in which the amount of nitrogen atoms derived from the amine compound group was 48 ppm ( ⁇ g / g), an amine compound group, and a solvent were obtained.
  • the mass ratio of the light emitting semiconductor material in the composition to the nitrogen atom in the amine compound group was 0.00145.
  • the mass ratio of the luminescent semiconductor material in the composition to the lead atom in the perovskite measured by ICP-MS was 0.0715.
  • the value of [(emission intensity derived from semiconductor material after 1 hour) / (emission intensity derived from semiconductor material immediately after mixing of semiconductor materials)] was 0.68.
  • the value of [(Full width at half maximum of light emission from semiconductor material after 1 hour)-(Full width at half maximum of light emission from semiconductor material immediately after mixing of semiconductor materials)] was 0.90 nm.
  • the value of [(emission intensity of emission from perovskite compound after 1 hour) / (emission intensity from perovskite compound immediately after mixing of semiconductor material)] was 1.0.
  • the emission spectrum was measured by mixing the dispersion composition having a nitrogen atom amount derived from the amine compound group of 48 ppm ( ⁇ g / g) with 2.25 mL of toluene and diluting the mixture with 0.01 mL. A solution obtained by mixing 2.99 mL of toluene was measured.
  • Example 2 The washed perovskite compound obtained in the same manner as in Example 1 was redispersed in toluene to obtain a dispersion liquid containing the perovskite compound.
  • concentration of the perovskite compound measured by ICP-MS and ion chromatography was 15000 ppm ( ⁇ g / g).
  • the nitrogen amount derived from the amine compound group and the molar ratio of Pb (N / Pb) contained in the above-mentioned dispersion containing perovskite were 0.3 as measured by XPS.
  • the amount of nitrogen derived from the amine compound group contained in the above-mentioned dispersion containing perovskite was 145 ppm ( ⁇ g / g) calculated from the amount of Nb / Pb measured by XPS and the amount of Pb measured by ICP-MS.
  • a dispersion composition containing the above-mentioned perovskite, a solvent, and an amine compound group 0.25 mL of a dispersion composition containing the above-mentioned perovskite, a solvent, and an amine compound group.
  • a dispersion composition containing InP and perovskite having a nitrogen atom content of 48 ppm ( ⁇ g / g) derived from the amine compound group, the amine compound group, and a solvent was 0.00145.
  • the mass ratio of the luminescent semiconductor material in the composition to the lead atom in the perovskite measured by ICP-MS was 0.0715.
  • the value of [(emission intensity derived from semiconductor material after 1 hour) / (emission intensity derived from semiconductor material immediately after mixing semiconductor material)] was 0.92.
  • the value of [(Full width at half maximum of light emission from semiconductor material after 1 hour)-(Full width at half maximum of light emission from semiconductor material immediately after mixing of semiconductor materials)] was 0.57 nm.
  • the value of [(emission intensity of emission from perovskite compound after 1 hour) / (emission intensity from perovskite compound immediately after mixing of semiconductor material)] was 0.87.
  • the emission spectrum was measured by mixing the dispersion composition having a nitrogen atom amount derived from the amine compound group of 48 ppm ( ⁇ g / g) with 2.25 mL of toluene and diluting the mixture with 0.01 mL. A solution obtained by mixing 2.99 mL of toluene was measured.
  • the amount of nitrogen derived from the amine compound group contained in the above-mentioned dispersion containing perovskite was measured by GC-MS, and the amount of Pb was measured by ICP-MS.
  • the molar ratio (N / Pb) of the amount of nitrogen and the amount of Pb was calculated from the obtained measured value, and it was 0.16.
  • the amount of nitrogen derived from the amine compound group contained in the above-mentioned dispersion containing perovskite was 78.6 ppm ( ⁇ g / g) as measured by GC-MS.
  • the value of [(emission intensity derived from semiconductor material after 1 hour) / (emission intensity derived from semiconductor material immediately after mixing of semiconductor materials)] was 0.75.
  • the value of [(Full width at half maximum of light emission from semiconductor material after 1 hour)-(Full width at half maximum of light emission from semiconductor material immediately after mixing of semiconductor materials)] was 0.59 nm.
  • the value of [(emission intensity of emission from perovskite compound after 1 hour) / (emission intensity from perovskite compound immediately after mixing of semiconductor material)] was 0.75.
  • the emission spectrum was measured by mixing the dispersion composition in which the amount of nitrogen atoms derived from the amine compound group was 26.2 ppm ( ⁇ g / g) with 2.25 mL of toluene, and then diluting the mixture with 0.01 mL. Then, a solution obtained by mixing 2.99 mL of toluene was measured.
  • Example 4 A dispersion containing perovskite was obtained by the same method as in Example 3. The amount of nitrogen derived from the amine compound group contained in the above-mentioned dispersion containing perovskite was measured by GC-MS, and the amount of Pb was measured by ICP-MS. The molar ratio (N / Pb) of the amount of nitrogen and the amount of Pb was calculated from the obtained measured value, and it was 0.16. The amount of nitrogen derived from the amine compound group contained in the above-mentioned dispersion containing perovskite was 78.6 ppm ( ⁇ g / g) as measured by GC-MS.
  • Polysilazane (AZNN-120-20, manufactured by Merck Performance Materials Co., Ltd.) was added to the above dispersion liquid, and the mixture was stirred for 1 hour with a magnetic stirrer to carry out a reaction.
  • Si / Pb (molar ratio) calculated from the amount of Pb and the amount of Si measured by ICP-MS was 15.9.
  • the value of [(emission intensity derived from semiconductor material after 1 hour) / (emission intensity derived from semiconductor material immediately after mixing of semiconductor materials)] was 0.82.
  • the value of [(FWHM of emission from semiconductor material after 1 hour)-(FWHM of emission from semiconductor material immediately after mixing of semiconductor materials)] was -0.16 nm.
  • the value of [(emission intensity of emission from perovskite compound after 1 hour) / (emission intensity from perovskite compound immediately after mixing of semiconductor material)] was 0.80.
  • the emission spectrum was measured by mixing the dispersion composition in which the amount of nitrogen atoms derived from the amine compound group was 26.2 ppm ( ⁇ g / g) with 2.25 mL of toluene, and then diluting the mixture with 0.01 mL. Then, a solution obtained by mixing 2.99 mL of toluene was measured.
  • the concentration of the perovskite compound measured by ICP-MS and ion chromatography was 15000 ppm ( ⁇ g / g). 0.25 mL of the dispersion liquid containing the above-mentioned perovskite was collected and mixed with 50 ⁇ L of oleylamine. The amount of nitrogen derived from the amine compound group and the molar ratio of Pb (N / Pb) contained in the above-mentioned dispersion containing perovskite were 21.1 as measured by XPS.
  • the amount of nitrogen derived from the amine compound group contained in the above-mentioned dispersion containing perovskite was 8573 ppm ( ⁇ g / g) calculated from the nitrogen atom / Pb measured by XPS and the amount of lead measured by ICP-MS.
  • 0.1 mL of a commercially available toluene dispersion of InP / ZnS (solid content of luminescent semiconductor material: 5%; emission wavelength: 630 nm) was added to the dispersion composition containing the perovskite, the solvent, and the amine compound group.
  • a dispersion liquid composition containing InP and perovskite having a nitrogen atom amount derived from the amine compound group of 7610 ppm ( ⁇ g / g), an amine compound group, and a solvent was obtained.
  • the mass ratio of nitrogen atoms contained in the amine compound group in the composition to the mass ratio of nitrogen atoms in the light emitting semiconductor material (nitrogen atom / (10) component) was 0.53.
  • the emission spectrum was measured by measuring the dispersion composition containing InP and the perovskite having a nitrogen atom content of 7610 ppm ( ⁇ g / g) derived from the amine compound group, the amine compound group, and the dispersion composition containing the solvent with 2.25 mL of toluene. After mixing and diluting, 0.01 mL of the solution was taken from the solution, and 2.99 mL of toluene was mixed to measure a solution.
  • the amount of nitrogen derived from the amine compound group contained in the above-mentioned dispersion liquid containing perovskite was 0 ppm ( ⁇ g / g) as measured by GC-MS.
  • the amount of nitrogen derived from the amine compound group and the molar ratio of Pb (N / Pb) contained in the above-mentioned dispersion containing the perovskite were measured by GC-MS, and the calculated amount of nitrogen derived from the amine compound group and ICP-MS The value was 0 calculated from the Pb amount measured by.
  • the value of [(emission intensity derived from semiconductor material after 1 hour) / (emission intensity derived from semiconductor material immediately after mixing of semiconductor materials)] was 0.84.
  • the value of [(FWHM of emission from semiconductor material after 1 hour)-(FWHM of emission from semiconductor material immediately after mixing of semiconductor materials)] was 1.29 nm.
  • the value of [(emission intensity of emission from perovskite compound after 1 hour) / (emission intensity from perovskite compound immediately after mixing of semiconductor material)] was 0.
  • the emission spectrum is measured by mixing the dispersion composition containing InP, perovskite, and a solvent with 2.25 mL of toluene, diluting the same, and further collecting 0.01 mL from the diluted solution to measure a solution containing 2.99 mL of toluene. did.
  • a resin composition can be obtained by forming the composition described in Experimental Examples 1 to 4 and Examples 1 to 4 into a sheet, and a film obtained by sandwiching the composition with two barrier films and sealing the film is provided on the light guide plate.
  • a blue light emitted from the blue light emitting diode placed on the end surface (side surface) of the light guide plate to the sheet through the light guide plate can be converted into green light or red light. .
  • a wavelength conversion material can be obtained by mixing the composition described in Experimental Examples 1 to 4 and Examples 1 to 4 with a resist and then removing the solvent. By arranging the obtained wavelength conversion material between the blue light emitting diode which is the light source and the light guide plate or in the subsequent stage of the OLED which is the light source, a backlight capable of converting the blue light of the light source into green light or red light is provided. To manufacture.
  • a titanium oxide dense layer is laminated on the surface of a fluorine-doped tin oxide (FTO) substrate, and a porous aluminum oxide layer is laminated thereon, and Experimental Examples 1 to 4 and Examples 1 to 4 are formed thereon.
  • FTO fluorine-doped tin oxide
  • Experimental Examples 1 to 4 and Examples 1 to 4 are formed thereon.
  • Spiro-OMeTAD 2,2-, 7,7-tetrakis- (N, N-di-p-methoxyphenylamine) 9,9-spirobifluorene
  • a hole transporting layer is laminated, and a silver (Ag) layer is laminated on it to manufacture a solar cell.
  • the composition of the present embodiment can be obtained by removing the solvent from the compositions of Experimental Examples 1 to 4 and Examples 1 to 4 and molding the composition. Then, a laser diode illumination that emits white light by converting blue light emitted from the blue light emitting diode to the composition into green light or red light is manufactured.
  • the composition of this embodiment can be obtained by removing the solvent of the composition described in Experimental Examples 1 to 4 and Examples 1 to 4 and molding.
  • a photoelectric conversion element (photodetection element) material used for a detection unit that detects light is manufactured.
  • the photoelectric conversion element material is used for a part of a living body such as an image detection part (image sensor) for a solid-state imaging device such as an X-ray imaging device and a CMOS image sensor, a fingerprint detection part, a face detection part, a vein detection part and an iris detection part. It is used in optical biosensors such as pulse oximeters that detect specific characteristics.

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Abstract

L'invention concerne une composition ayant des propriétés d'émission de lumière, qui contient des composants (1) et (2) et au moins un composant choisi dans le groupe constitué par les composants (3), (4) et (4-1), le rapport du nombre de moles d'atomes d'azote contenus dans le composant (2) au nombre de moles de B contenu dans Le composant (1) étant supérieur à 0 et inférieur ou égal à 0,55. Composant (1) : est un composé pérovskite contenant A, B et X en tant qu'éléments constitutifs. (A représente un composant situé à chaque sommet d'un hexaèdre centré sur B dans une structure cristalline de type pérovskite, et est un cation monovalent. X représente un composant situé à chaque sommet d'un octaèdre centré sur B dans la structure cristalline de type pérovskite, et est au moins un anion choisi dans le groupe constitué par un ion halogénure et un ion thiocyanate. B représente un composant situé au centre de chacun d'un hexaèdre dans lequel A est situé à chaque sommet et d'un octaèdre dans lequel X est situé à chaque sommet dans une structure cristalline de type pérovskite, et est un ion métallique). Composant (2) : un composé représenté par la formule : ClNmHn, un ion d'un composé représenté par la formule : ClNmHn, ou un sel d'un ion d'un composé représenté par la formule : ClNmHn (où l, m et n représentent indépendamment un nombre entier). Composant (3) : un solvant. Composant (4) : un composé polymérisable. Composant (4-1) : un polymère.
PCT/JP2019/042100 2018-10-26 2019-10-28 Composition, film, structure de stratifié, dispositif électroluminescent et dispositif d'affichage WO2020085514A1 (fr)

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CN113611807A (zh) * 2021-07-12 2021-11-05 深圳大学 蓝光钙钛矿发光二极管及其制备方法

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