WO2014208356A1 - Film optique et dispositif d'émission de lumière - Google Patents

Film optique et dispositif d'émission de lumière Download PDF

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Publication number
WO2014208356A1
WO2014208356A1 PCT/JP2014/065688 JP2014065688W WO2014208356A1 WO 2014208356 A1 WO2014208356 A1 WO 2014208356A1 JP 2014065688 W JP2014065688 W JP 2014065688W WO 2014208356 A1 WO2014208356 A1 WO 2014208356A1
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WIPO (PCT)
Prior art keywords
semiconductor nanoparticles
semiconductor
optical film
resin
polysilazane
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PCT/JP2014/065688
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English (en)
Japanese (ja)
Inventor
宏司 高木
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コニカミノルタ株式会社
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Priority to JP2015523976A priority Critical patent/JPWO2014208356A1/ja
Publication of WO2014208356A1 publication Critical patent/WO2014208356A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/206—Filters comprising particles embedded in a solid matrix
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/0001—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings specially adapted for lighting devices or systems
    • G02B6/0011—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings specially adapted for lighting devices or systems the light guides being planar or of plate-like form
    • G02B6/0033—Means for improving the coupling-out of light from the light guide
    • G02B6/005—Means for improving the coupling-out of light from the light guide provided by one optical element, or plurality thereof, placed on the light output side of the light guide
    • G02B6/0051—Diffusing sheet or layer
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
    • G02F1/1336—Illuminating devices
    • G02F1/133615—Edge-illuminating devices, i.e. illuminating from the side
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/712—Weather resistant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2551/00—Optical elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
    • G02F1/1336—Illuminating devices
    • G02F1/133614—Illuminating devices using photoluminescence, e.g. phosphors illuminated by UV or blue light
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F2202/00—Materials and properties
    • G02F2202/36—Micro- or nanomaterials

Definitions

  • the present invention relates to an optical film and a light emitting device.
  • the present invention relates to an optical film having durability capable of suppressing deterioration of semiconductor nanoparticles due to oxygen or the like over a long period of time and excellent in transparency, and a light emitting device including the optical film.
  • semiconductor nanoparticles have gained commercial interest due to their variable electronic properties.
  • Semiconductor nanoparticles are, for example, biomarkers, solar power generation, catalysis, bioimaging, light emitting diodes (hereinafter abbreviated as LEDs), general spatial illumination, and electroluminescent displays. It is expected to be used in various fields.
  • the amount of light incident on a liquid crystal display (hereinafter abbreviated as LCD) by irradiating the semiconductor nanoparticles with LED light to emit light.
  • LCD liquid crystal display
  • the conventional technique of covering the surface of the semiconductor nanoparticles with silica or glass, or the method of dispersing them in an inorganic matrix can obtain oxygen barrier performance, but the silica nanoparticles of the semiconductor nanoparticles are formed.
  • the dispersibility in the layer is lowered, the transparency is lowered, or the oxygen blocking performance is lowered due to the influence of the external environment, the brightness is deteriorated, etc. It was insufficient in terms of durability.
  • Patent Document 5 proposes a method of dispersing and holding semiconductor nanoparticles in a transparent resin layer.
  • the method proposed here is insufficient in terms of durability, for example, the luminance is deteriorated due to a decrease in oxygen barrier performance due to the influence of the external environment.
  • the present invention has been made in view of the above problems, and its solution is an optical film having durability that can prevent deterioration of semiconductor nanoparticles due to oxygen or the like over a long period of time and having excellent transparency. It is to provide a light emitting device including the optical film.
  • the present inventor contains, as a semiconductor nanoparticle layer, at least one compound selected from polysilazane and a modified polysilazane and semiconductor nanoparticles coated with a resin. It has been found that an optical film having excellent durability capable of preventing the deterioration of semiconductor nanoparticles due to oxygen or the like over a long period of time and further excellent in transparency can be obtained by constituting the present invention.
  • An optical film having a substrate and a semiconductor nanoparticle layer provided on the substrate, The optical film, wherein the semiconductor nanoparticle layer contains at least one selected from semiconductor nanoparticles coated with a resin, polysilazane and a polysilazane modified body that disperses and holds the semiconductor nanoparticles.
  • the semiconductor nanoparticle layer contains the polysilazane modified body, and the polysilazane modified body is formed by irradiating the polysilazane with vacuum ultraviolet rays, and at least one selected from silicon oxide, silicon nitride, and silicon oxynitride 2.
  • the semiconductor nanoparticle layer having two or more layers, wherein the two or more semiconductor nanoparticle layers contain semiconductor nanoparticles having different emission wavelengths, respectively.
  • the optical film as described in any one of the above.
  • a light emitting device comprising the optical film according to any one of items 1 to 6.
  • an optical film having excellent luminous efficiency and excellent durability capable of suppressing deterioration of semiconductor nanoparticles due to oxygen or the like over a long period of time and having excellent transparency and the optical film are provided.
  • the light emitting device can be provided.
  • the polysilazane and the polysilazane modified body which are constituent elements of the present invention, not only have an oxygen-blocking property but also an oxygen-absorbing performance, so that it is possible to effectively reduce oxygen in contact with semiconductor nanoparticles. As a result, it is speculated that sufficient durability (oxidation resistance) can be secured.
  • the polysilazane and the modified polysilazane can further improve the oxygen barrier property by light irradiation such as vacuum ultraviolet irradiation.
  • the semiconductor nanoparticles in the polysilazane or polysilazane modified body are contained. It is presumed that the optical film and the light-emitting device, which are greatly improved in dispersibility and excellent in transparency, luminous efficiency and durability, can be obtained.
  • the optical film of the present invention is an optical film having a base material and a semiconductor nanoparticle layer provided on the base material, wherein the semiconductor nanoparticle layer is coated with a resin, It is characterized by containing at least one compound selected from polysilazane and a modified polysilazane as a binder for dispersing and holding semiconductor nanoparticles (hereinafter also referred to as “quantum dots”).
  • Quantum dots semiconductor nanoparticles
  • the semiconductor nanoparticle layer contains the polysilazane modified product, and the polysilazane modified product applies a vacuum ultraviolet ray to the polysilazane from the viewpoint of more manifesting the intended effect of the present invention.
  • a compound containing at least one selected from silicon oxide, silicon nitride, and silicon oxynitride formed by irradiation is preferable from the viewpoint of obtaining higher-order oxygen barrier properties for semiconductor nanoparticles. .
  • the fact that the semiconductor nanoparticles have a core-shell structure can suppress the aggregation of the semiconductor nanoparticles, can further increase dispersibility, and can improve luminance efficiency. Good.
  • the resin is an ultraviolet curable resin from the viewpoint of easy manufacture of the optical film.
  • the resin is a water-soluble resin from the viewpoint that an optical film can be easily manufactured with simple manufacturing equipment.
  • two or more semiconductor nanoparticle layers are provided, and the two or more semiconductor nanoparticle layers each contain semiconductor nanoparticles having different emission wavelengths, so that various optical emissions can be obtained as an optical film. It is preferable from a viewpoint which can be obtained.
  • ⁇ is used to mean that the numerical values described before and after it are included as a lower limit value and an upper limit value.
  • the optical film of the present invention comprises a base material, at least one compound selected from polysilazane and a modified polysilazane as a binder on the base material, and semiconductor nanoparticles whose particle surfaces are coated with a resin in the binder. It is characterized by having a semiconductor nanoparticle layer dispersed and contained.
  • FIG. 1 is a schematic cross-sectional view showing an example of the configuration of the optical film of the present invention.
  • an optical film 11 of the present invention has a configuration in which a semiconductor nanoparticle layer 13 is laminated on a base material 12.
  • the semiconductor nanoparticle layer 13 according to the present invention has a configuration in which the semiconductor nanoparticles 15 whose surfaces are coated with the resin 16 are dispersed in the polysilazane or polysilazane modified body 14 as a binder.
  • the base material applicable to the optical film of the present invention is not particularly limited as long as it has optical transparency, such as glass and plastic.
  • Examples of the material preferably used as the base material having translucency include glass, quartz, and a resin film. Particularly preferred is a resin film from the viewpoint of imparting flexibility to the optical film.
  • the light transmittance of the substrate as used in the present invention means that the visible light transmittance is 60% or more, preferably 80% or more, more preferably 90% or more.
  • the thickness of the substrate is not particularly limited, but is generally in the range of 15 to 300 ⁇ m, preferably in the range of 15 to 200 ⁇ m, and more preferably in the range of 18 to 150 ⁇ m. .
  • polyesters such as polyethylene terephthalate (PET) and polyethylene naphthalate (PEN), cellulose diacetate, cellulose triacetate (TAC), cellulose acetate butyrate, cellulose acetate propionate (CAP), and cellulose acetate.
  • PET polyethylene terephthalate
  • PEN polyethylene naphthalate
  • TAC cellulose triacetate
  • CAP cellulose acetate propionate
  • Cellulose esters such as phthalate and cellulose nitrate or derivatives thereof, polyethylene, polypropylene, cellophane, polyvinylidene chloride, polyvinyl alcohol, polyethylene vinyl alcohol, syndiotactic polystyrene, polycarbonate, norbornene resin, polymethylpentene, polyether ketone, Polyimide, polyethersulfone (PES), polyphenylene sulfide, polysulfone , Polyetherimide, polyetherketoneimide, polyamide, fluororesin, nylon, polymethylmethacrylate, acrylic or polyarylates, cyclone resins such as Arton (trade name, manufactured by JSR) or Appel (trade name, manufactured by Mitsui Chemicals) Etc.
  • PES polyethersulfone
  • Polyetherimide polyetherketoneimide
  • polyamide fluororesin
  • nylon polymethylmethacrylate
  • cyclone resins such as Arton (trade
  • membrane which consists of an inorganic substance, an organic substance, or both may be formed in the surface of the said resin film.
  • a water vapor permeability (25 ⁇ 0.5 ° C., relative humidity (90 ⁇ 2)% RH) measured by a method according to JIS K 7129-1992 is 0.01 g.
  • the oxygen permeability measured by a method according to JIS K 7126-1987 is 1 ⁇ 10 ⁇ 3 ml / (m 2 More preferably, it is a high gas barrier film having a water vapor permeability of 1 ⁇ 10 ⁇ 5 g / (m 2 ⁇ 24 h) or less.
  • any material that has a function of suppressing intrusion of semiconductor nanoparticles such as moisture and oxygen may be used.
  • silicon oxide, silicon dioxide, silicon nitride, oxynitride Silicon or the like can be used.
  • the method for forming the gas barrier film is not particularly limited.
  • a plasma CVD method, a laser CVD method, a thermal CVD method, a coating method, or the like can be used, but an atmospheric pressure plasma polymerization method as described in JP-A-2004-68143 is preferable.
  • the semiconductor nanoparticle layer according to the present invention comprises at least one compound selected from polysilazane and a modified polysilazane and semiconductor nanoparticles coated with a resin.
  • the optical film of the present invention is characterized by having at least one semiconductor nanoparticle layer according to the present invention, but the semiconductor nanoparticle layer may have a structure in which two or more layers are provided. . In the case of having two or more semiconductor nanoparticle layers, it is preferable that each semiconductor nanoparticle layer contains semiconductor nanoparticles having different emission wavelengths.
  • a coating solution for forming a semiconductor nanoparticle layer containing a semiconductor nanoparticle coated with a polysilazane modified material and a resin is applied on a substrate, followed by drying treatment.
  • the method of forming can be mentioned.
  • the coating method is not particularly limited, and a conventionally known wet coating method can be appropriately selected and applied.
  • Specific wet methods include, for example, spin coating methods, roller coating methods, flow coating methods, ink jet methods, spray coating methods, printing methods, dip coating methods, cast film forming methods, bar coating methods, gravure printing methods, and the like. Is mentioned.
  • any solvent can be used as long as it does not react with semiconductor nanoparticles, polysilazane, modified polysilazane, and the like. It can be used even if it exists.
  • a method for forming the semiconductor nanoparticle layer after applying a semiconductor nanoparticle layer forming coating solution containing semiconductor nanoparticles coated with polysilazane and resin on a substrate, a method described later, for example, Alternatively, a method of forming a semiconductor nanoparticle layer by performing a modification treatment in which a part or all of polysilazane is modified into a polysilazane modified body by irradiation with excimer light or the like can also be used.
  • the semiconductor nanoparticle layer preferably further contains a resin material, and more preferably contains an ultraviolet curable resin or a water-soluble resin. If the semiconductor nanoparticle layer contains an ultraviolet curable resin, that is, if the semiconductor nanoparticle layer forming coating solution contains an ultraviolet curable resin, apply the semiconductor nanoparticle layer forming coating solution.
  • the coating layer thus formed is subjected to ultraviolet irradiation treatment.
  • the ultraviolet irradiation treatment may also serve as a modification treatment for modifying the polysilazane described above. Details of the ultraviolet curable resin and the water-soluble resin will be described later.
  • the thickness of the semiconductor nanoparticle layer is not particularly limited, but is approximately in the range of 20 to 300 ⁇ m, preferably in the range of 50 to 200 ⁇ m, and more preferably in the range of 80 to 140 ⁇ m. is there.
  • One feature of the semiconductor nanoparticle layer constituting the optical film of the present invention is that it contains semiconductor nanoparticles whose surface is coated with a resin. That is, the semiconductor nanoparticles are contained in the coating solution for forming the semiconductor nanoparticle layer.
  • the semiconductor nanoparticle according to the present invention refers to a particle having a predetermined size, which is composed of a crystal of a semiconductor material and has a quantum confinement effect, and whose particle diameter is in the range of several nanometers to several tens of nanometers. In this case, the quantum dot effect shown below is obtained.
  • the particle diameter of the semiconductor nanoparticles according to the present invention is preferably in the range of 1 to 20 nm, more preferably in the range of 1 to 10 nm.
  • the energy level E of such semiconductor nanoparticles is generally expressed by the following formula (1) when the Planck constant is “h”, the effective mass of electrons is “m”, and the radius of the semiconductor nanoparticles is “R”. expressed.
  • the energy level E (hereinafter also referred to as a band gap) of the semiconductor nanoparticles increases in proportion to the radius “R ⁇ 2 ” of the semiconductor nanoparticles, so-called quantum dots.
  • the band gap value of the semiconductor nanoparticles can be controlled by controlling and defining the particle diameter of the semiconductor nanoparticles. That is, by controlling and defining the particle diameter of the semiconductor nanoparticles, it is possible to impart diversity not found in ordinary atoms. Therefore, it can be excited by light, or converted into light having a desired wavelength and emitted.
  • such a light-emitting semiconductor nanoparticle material is defined as “semiconductor nanoparticle” or quantum dot.
  • the average particle diameter of the semiconductor nanoparticles is in the range of several nanometers to several tens of nanometers, and is set to an average particle diameter corresponding to each target emission color.
  • the average particle size of the semiconductor nanoparticles is preferably set within a range of 3.0 to 20 nm.
  • the average particle size of the semiconductor nanoparticles is selected.
  • the diameter is preferably set in the range of 1.5 to 10 nm.
  • the average particle diameter of the semiconductor nanoparticles is preferably set in the range of 1.0 to 3.0 nm. .
  • a known method can be used. For example, a method of observing semiconductor nanoparticles using a transmission electron microscope (TEM) and obtaining the number average particle size of the particle size distribution therefrom, or a method of obtaining an average particle size using an atomic force microscope (AFM)
  • TEM transmission electron microscope
  • AFM atomic force microscope
  • a particle size measuring apparatus using a dynamic light scattering method for example, a method using a “Zeta Sizer Nano Series Zeta Sizer Nano ZS” manufactured by Malvern, Inc. can be used.
  • the average aspect ratio (major axis diameter / minor axis diameter) value is preferably in the range of 1.0 to 2.0, more preferably 1.0. Is within the range of 1.7.
  • the average aspect ratio (major axis diameter / minor axis diameter) of the semiconductor nanoparticles according to the present invention can be determined by measuring the major axis diameter and the minor axis diameter using, for example, an atomic force microscope (AFM). it can. The number of particles to be measured is 300 or more, and the average value is calculated.
  • the addition amount of the semiconductor nanoparticles is preferably in the range of 0.01 to 50% by mass, and in the range of 0.5 to 30% by mass, where 100% by mass of all the constituent materials of the semiconductor nanoparticle layer is taken. Is more preferable, and most preferably in the range of 2.0 to 25% by mass. If the addition amount is 0.01% by mass or more, sufficient luminance efficiency can be obtained, and if it is 50% by mass or less, an appropriate inter-particle distance of the semiconductor nanoparticles can be maintained, and the quantum size effect can be sufficiently obtained. Can be expressed.
  • Constituent material of semiconductor nanoparticles examples include a simple substance of Group 14 element of the periodic table such as carbon, silicon, germanium and tin, a simple substance of Group 15 element of the periodic table such as phosphorus (black phosphorus), and selenium. And simple substances of Group 16 elements of the periodic table such as tellurium.
  • compounds composed of a plurality of Group 14 elements of the periodic table such as silicon carbide (SiC), for example, tin (IV) (SnO 2 ), tin (II, IV) (Sn (II) Sn (IV) S 3 ), tin sulfide (IV) (SnS 2 ), tin sulfide (II) (SnS), tin selenide (II) (SnSe), tin telluride (II) (SnTe), lead sulfide (II) (PbS) , Lead selenide (II) (PbSe), lead telluride (II) (PbTe) periodic table group 14 element and periodic table group 16 element compound, boron nitride (BN), boron phosphide (BP ), Boron arsenide (BAs), aluminum nitride (AlN), aluminum phosphide (AlP), aluminum arsenide (A
  • Al 2 S 3 aluminum sulfide
  • Al 2 Se 3 aluminum selenide
  • Ga 2 S 3 gallium sulfide
  • Ga 2 Se 3 gallium selenide
  • Periods of gallium telluride (Ga 2 Te 3 ) indium oxide (In 2 O 3 ), indium sulfide (In 2 S 3 ), indium selenide (In 2 Se 3 ), indium telluride (In 2 Te 3 ), etc.
  • Compounds of Group 13 elements and Group 16 elements of the periodic table include compounds of thallium chloride (I) (TlCl), thallium bromide (I) ( LBR), include compounds of thallium iodide (I) (TlI) periodic table group 13 elements and the periodic table Group 17 element such.
  • Compounds of elements and group 17 elements of the periodic table compounds of group 10 elements of the periodic table and group 16 elements of the periodic table such as nickel oxide (II) (NiO), cobalt (II) oxide (CoO), cobalt sulfide (II) (CoS) periodic table group 9 element and periodic table group 16 element compound, triiron tetroxide (Fe 3 O 4 ), iron sulfide (II) (FeS) periodic table 8
  • a compound of a group element and a group 16 element of the periodic table, a compound of a group 7 element of the periodic table and a group 16 element of the periodic table such as manganese oxide (II) (MnO), molybdenum sulfide (IV) (MoS 2 ), Compounds of periodic table group 6 elements and periodic table group 16 elements such as tungsten oxide (IV) (WO 2 );
  • Compound of periodic table group 5 element and periodic table group 16 element such as vanadium oxide (II) (VO), van
  • a compound of a periodic table group 14 element and a periodic table group 16 element such as SnS 2 , SnS, SnSe, SnTe, PbS, PbSe, PbTe, GaN, GaP, GaAs, GaSb, InN, InP, III-V group compound semiconductors such as InAs and InSb, Ga 2 O 3 , Ga 2 S 3 , Ga 2 Se 3 , Ga 2 Te 3 , In 2 O 3 , In 2 S 3 , In 2 Se 3 , In 2 Te
  • II-VI compounds such as ZnO, ZnS, ZnSe, ZnTe, CdO, CdS, CdSe, CdTe, HgO, HgS, HgSe, HgTe semiconductor, As 2 O 3, As 2 S 3, As 2 Se 3, As 2 Te 3, Sb 2 O 3, Sb 2 S 3, Sb 2 S 3, Sb
  • these substances do not contain highly toxic negative elements, they have excellent resistance to environmental pollution and safety to living organisms. In addition, a pure spectrum can be stably obtained in the visible light region, so that luminescence is achieved. It is advantageous for forming a device.
  • these materials CdSe, ZnSe, and CdS are particularly preferable in terms of light emission stability.
  • semiconductor nanoparticles of ZnO and ZnS are preferred from the viewpoints of luminous efficiency, high refractive index, safety and economy.
  • said material may be used by 1 type and may be used in combination of 2 or more type.
  • the semiconductor nanoparticles described above can be doped with a small amount of various elements as impurities as necessary. By adding such a doping substance, the light emission characteristics can be greatly improved.
  • the emission wavelength (band gap) as used in the present invention is the band gap (eV) in the semiconductor nanoparticles, and the energy difference between the valence band and the conduction band.
  • nm 1240 / band gap (eV).
  • the band gap (eV) of the semiconductor nanoparticles can be measured using a Tauc plot.
  • the Tauc plot which is one of the optical scientific measurement methods of the band gap (eV), will be described.
  • the maximum wavelength of the emission spectrum can be simply used as an index of the band gap.
  • the surface of the semiconductor nanoparticles is preferably coated with an inorganic coating layer or a coating composed of an organic ligand. That is, the surface of the semiconductor nanoparticle has a core-shell structure having a core region composed of a semiconductor nanoparticle material and a shell region composed of an inorganic coating layer or an organic ligand. preferable.
  • This core / shell structure is preferably formed of at least two kinds of compounds, and may form a gradient structure (gradient structure) with two or more kinds of compounds.
  • gradient structure gradient structure
  • aggregation of the semiconductor nanoparticles in the coating liquid can be effectively prevented, the dispersibility of the semiconductor nanoparticles can be improved, the luminance efficiency is improved, and the optical film of the present invention is used.
  • the light emitting device is continuously driven, the occurrence of color misregistration can be suppressed.
  • stable emission characteristics can be obtained due to the presence of the coating layer (shell region).
  • the surface of the semiconductor nanoparticles is coated with the coating layer (shell region), a surface modifier as described later can be reliably supported in the vicinity of the surface of the semiconductor nanoparticles.
  • the thickness of the coating layer (shell region) is not particularly limited, but is preferably in the range of 0.1 to 10 nm, and more preferably in the range of 0.1 to 5 nm.
  • a semiconductor nanoparticle can control the emission color by its average particle diameter, and if the thickness of the coating layer is within the above range, the thickness of the coating corresponds to the number of atoms.
  • the thickness is less than one semiconductor nanoparticle, the semiconductor nanoparticle can be filled with high density, and a sufficient amount of light emission can be obtained.
  • the presence of the coating can suppress non-luminous electron energy transfer due to defects existing on the particle surfaces of the core particles and electron traps on the dangling bonds, thereby suppressing a decrease in quantum efficiency.
  • the production method in a high vacuum environment includes a molecular beam epitaxy method, a CVD method, and the like.
  • a raw material aqueous solution is used, for example, an alkane such as n-heptane, n-octane, or isooctane.
  • a reverse micelle method in which a crystal is grown in a reverse micelle phase in a non-polar organic solvent such as aromatic hydrocarbon such as benzene, toluene, xylene, etc.
  • Examples include a hot soap method in which crystals are grown by injecting into a phase organic medium, and a solution reaction method involving crystal growth at a relatively low temperature using an acid-base reaction as a driving force, as in the hot soap method. Any method can be applied from these production methods, and among these, the liquid phase production method is preferable.
  • the organic surface modifier which exists on the surface is called an initial stage surface modifier.
  • the initial surface modifier in the hot soap method include trialkylphosphines, trialkylphosphine oxides, alkylamines, dialkyl sulfoxides, alkanephosphonic acid and the like. These initial surface modifiers are preferably exchanged for the following functional surface modifiers by an exchange reaction.
  • the initial surface modifier such as trioctyl phosphine oxide obtained by the hot soap method described above is subjected to an exchange reaction performed in a liquid phase containing a functional surface modifier, and the following (2) It can be exchanged for the functional surface modifier shown in FIG.
  • the semiconductor nanoparticle according to the present invention is characterized in that its surface is coated with a resin. Before coating with a resin, a surface modifier is applied to the semiconductor nanoparticle. It may be given.
  • the dispersion stability of the semiconductor nanoparticles in the coating solution for forming the semiconductor nanoparticle layer can be improved.
  • the surface of the semiconductor nanoparticles is attached to the surface of the semiconductor nanoparticles, so that the shape of the formed semiconductor nanoparticles becomes high in sphericity, and the particle size distribution of the semiconductor nanoparticles Can be kept narrow, and therefore can be made particularly excellent.
  • the functional surface modifier that can be applied in the present invention may be those directly attached to the surface of the semiconductor nanoparticles, or those attached via the shell, that is, the surface modifier is directly attached. May be a shell that is not in contact with the core of the semiconductor nanoparticles.
  • Polyoxyethylene alkyl ethers for example, polyoxyethylene lauryl ether, polyoxyethylene stearyl ether, polyoxyethylene oleyl ether, etc.
  • Trialkylphosphines For example, tripropylphosphine, tributylphosphine, trihexylphosphine, trioctylphosphine, etc.
  • Polyoxyethylene alkylphenyl ethers for example, polyoxyethylene n-octylphenyl ether, polyoxyethylene n-nonylphenyl ether, etc.
  • Tertiary amines for example, tri (n-hexyl) amine, tri (n-octyl) amine, tri (n-decyl) amine, etc.
  • Organophosphorus compounds for example, tripropylphosphine oxide, tributylphosphine oxide, trihexylphosphine oxide, trioctylphosphine oxide, tridecylphosphine oxide, etc.
  • Polyethylene glycol diesters for example, polyethylene glycol dilaurate, polyethylene glycol distearate, etc.
  • Organic nitrogen compounds For example, nitrogen-containing aromatic compounds of pyridine, lutidine, collidine, quinolines, etc.
  • Aminoalkanes for example, hexylamine, octylamine, decylamine, dodecylamine, tetradecylamine, hexadecylamine, octadecylamine, etc.
  • Dialkyl sulfides for example, dibutyl sulfide
  • Dialkyl sulfoxides for example, dimethyl sulfoxide, dibutyl sulfoxide, etc.
  • Organic sulfur compounds For example, sulfur-containing aromatic compounds such as thiophene, etc. 12
  • Higher fatty acids For example, palmitic acid, stearic acid, oleic acid, etc.
  • the surface modifier is a substance that is coordinated and stabilized by the fine particles of the semiconductor nanoparticles in a high-temperature liquid phase.
  • polysilazane described later can also be used as a surface modifier.
  • the size (average particle diameter) of the semiconductor nanoparticles is preferably in the range of 1 to 20 nm.
  • the size of the semiconductor nanoparticles referred to in the present invention is composed of a core region composed of a semiconductor nanoparticle material, a shell region composed of an inert inorganic coating layer or an organic ligand, and a surface modifier. Represents the total size. If the surface modifier or shell is not included, the size does not include it.
  • the semiconductor nanoparticles according to the present invention are characterized in that their surfaces are coated with a resin, and it is preferable that the resin is a transparent resin. is there.
  • the semiconductor nanoparticles coated with the resin according to the present invention may be either in a state having the surface modifier on the surface or in a state having no surface modifier.
  • the transparent resin referred to in the present invention means a resin having optical transparency, and more specifically, the visible light transmittance is 60% or more, preferably 80% or more, more preferably 90%. That's it. Therefore, the transparent resin referred to in the present invention is a resin having the above transmittance in the visible light region, and the transparent resin covering the surface of the semiconductor nanoparticles according to the present invention is not limited as long as it satisfies the above conditions. In particular, an ultraviolet curable resin or a water-soluble resin is preferable.
  • UV curable resin In the present invention, it is one of preferred embodiments that the surface of the semiconductor nanoparticles is coated with an ultraviolet curable resin.
  • Examples of the ultraviolet curable resin applicable to the present invention include radical polymerization such as an ultraviolet curable urethane acrylate resin, an ultraviolet curable polyester acrylate resin, an ultraviolet curable epoxy acrylate resin, and an ultraviolet curable polyol acrylate resin.
  • a cationic polymerizable resin such as a functional resin or an ultraviolet curable epoxy resin is preferably used.
  • an ultraviolet curable acrylate resin which is a radical polymerizable resin is preferable.
  • UV curable urethane acrylate resins are generally obtained by reacting a polyester polyol with an isocyanate monomer or a prepolymer, and further adding 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate (hereinafter referred to as methacrylate to the acrylate). It can be easily obtained by reacting an acrylate monomer having a hydroxy group such as 2-hydroxypropyl acrylate. For example, those described in JP-A-59-151110 can be used. Specifically, a mixture of 100 parts Unidic 17-806 (manufactured by DIC Corporation) and 1 part of Coronate L (manufactured by Nippon Polyurethane Corporation) is preferably used.
  • UV curable polyester acrylate resin examples include those that are easily formed when 2-hydroxyethyl acrylate and 2-hydroxy acrylate monomers are generally reacted with polyester polyol. No. 151112 can be used.
  • ultraviolet curable epoxy acrylate resin examples include an epoxy acrylate oligomer, a reactive diluent and a photopolymerization initiator added to the oligomer, and a reaction product. Those described in JP-A No. 1-105738 can be used.
  • UV curable polyol acrylate resins include trimethylolpropane triacrylate, ditrimethylolpropane tetraacrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate, alkyl-modified dipentaerythritol pentaacrylate, etc. Can be mentioned.
  • polymethyl methacrylate and polylauryl methacrylate obtained by polymerizing methyl methacrylate or lauryl methacrylate using ultraviolet rays are also classified as ultraviolet curable resins according to the present invention.
  • the photopolymerization initiator used for forming these ultraviolet curable resins include benzoin and its derivatives, acetophenone, benzophenone, hydroxybenzophenone, Michler's ketone, ⁇ -amyloxime ester, thioxanthone, and derivatives thereof. Can do. You may use with a photosensitizer.
  • the photopolymerization initiator can also be used as a photosensitizer. Further, when an epoxy acrylate photopolymerization initiator is used, a sensitizer such as n-butylamine, triethylamine, tri-n-butylphosphine can be used.
  • the photopolymerization initiator or photosensitizer used in the ultraviolet curable resin composition is in the range of 0.1 to 15 parts by mass, preferably in the range of 1 to 10 parts by mass, per 100 parts by mass of the composition. is there.
  • the resin coverage when the resin is coated on the surface of the semiconductor nanoparticles according to the present invention is not particularly limited, but when the total mass of the semiconductor nanoparticles coated with the resin is 100% by mass
  • the ratio of the resin to be coated is preferably in the range of 5 to 50% by mass, more preferably in the range of 10 to 35% by mass, and still more preferably in the range of 15 to 30% by mass. is there.
  • an ultraviolet curable resin is added to the solution containing the semiconductor nanoparticles while the surface of the semiconductor nanoparticles is irradiated with ultraviolet rays.
  • a method of forming a resin on the surface of the semiconductor nanoparticle by coating the curable resin and then subjecting the semiconductor nanoparticle coated with the ultraviolet curable resin to UV curing by ultraviolet irradiation, or UV curing on the surface of the semiconductor nanoparticle.
  • UV curable resin is applied to the particle surface by a solution polymerization method in a solution in which semiconductor nanoparticles are present, or after applying a functional resin using a spray-type wet coating apparatus such as a spray coater.
  • a spray-type wet coating apparatus such as a spray coater.
  • the method include a method of preparing semiconductor nanoparticles coated with a resin by performing UV curing after coating.
  • the prepared semiconductor nanoparticles coated with the resin are, for example, focused ion beam (FB-) manufactured by Hitachi High-Technologies. 2000A), a cross section is processed, and a surface passing through the vicinity of the particle center is cut out. Next, by observing the exposed cut surface of the center line with an electron microscope, the presence or absence of the coating resin, the thickness of the coated resin layer, and the ratio of the coated resin to the entire particles can be determined.
  • FB- focused ion beam
  • a cross section is processed by a focused ion beam (FB-2000A) manufactured by Hitachi High-Technologies, and a surface passing near the particle center is cut out. Then, from the cut surface, it can also be obtained by performing elemental analysis using STEM-EDX (HD-2000) manufactured by Hitachi High-Technologies, and measuring the composition distribution of the resin component and the semiconductor nanoparticle component.
  • FB-2000A focused ion beam
  • HD-2000 STEM-EDX
  • any light source that generates ultraviolet rays can be used without limitation.
  • a low pressure mercury lamp, a medium pressure mercury lamp, a high pressure mercury lamp, an ultrahigh pressure mercury lamp, a carbon arc lamp, a metal halide lamp, a xenon lamp, or the like can be used.
  • the irradiation conditions vary depending on individual irradiation light source, the irradiation amount of ultraviolet rays is usually within the range of 5 ⁇ 500mJ / cm 2, preferably in the range of 5 ⁇ 150mJ / cm 2.
  • Water-soluble resin> In the present invention, it is also a preferred embodiment to use a water-soluble resin as the resin for coating the semiconductor nanoparticles.
  • the water-soluble resin applicable to the present invention is not particularly limited, but polyvinyl alcohol resins, gelatin, celluloses, thickening polysaccharides, and resins having reactive functional groups can be used. Of these, it is preferable to use a polyvinyl alcohol-based resin.
  • the water-soluble in the present invention means a compound in which 1% by mass or more, preferably 3% by mass or more dissolves in an aqueous medium.
  • polyvinyl alcohol resin examples include, in addition to normal polyvinyl alcohol (unmodified polyvinyl alcohol) obtained by hydrolysis of polyvinyl acetate, cation-modified polyvinyl alcohol having a terminal cation-modified, anion Anionic modified polyvinyl alcohol having a functional group, modified polyvinyl alcohol modified with acrylic, reactive polyvinyl alcohol (for example, “Gosefimer Z” manufactured by Nihon Gosei Co., Ltd.), vinyl acetate resin (for example, “Kuraray Co., Ltd.” "Exeval”) is also included.
  • These polyvinyl alcohol-based resins can be used in combination of two or more different polymerization degrees and different types of modification.
  • silanol-modified polyvinyl alcohol having a silanol group for example, “R-1130” manufactured by Kuraray Co., Ltd.
  • silanol-modified polyvinyl alcohol having a silanol group for example, “R-1130” manufactured
  • Examples of the cation-modified polyvinyl alcohol include primary to tertiary amino groups and quaternary ammonium groups as described in JP-A No. 61-10383.
  • Anion-modified polyvinyl alcohol is described in, for example, polyvinyl alcohol having an anionic group as described in JP-A-1-206088, JP-A-61-237681 and JP-A-63-307979.
  • examples thereof include a copolymer of vinyl alcohol and a vinyl compound having a water-soluble group, and a modified polyvinyl alcohol having a water-soluble group as described in JP-A-7-285265.
  • Nonionic modified polyvinyl alcohol includes, for example, a polyvinyl alcohol derivative in which a polyalkylene oxide group is added to a part of vinyl alcohol as described in JP-A-7-9758, and JP-A-8-25795.
  • the block copolymer of the vinyl compound and vinyl alcohol which have the described hydrophobic group is mentioned.
  • Polyvinyl alcohol can be used in combination of two or more different degrees of polymerization and different types of modification.
  • vinyl acetate resins examples include Exeval (trade name: manufactured by Kuraray Co., Ltd.) and Nichigo G polymer (trade name: manufactured by Nippon Synthetic Chemical Industry Co., Ltd.).
  • the polymerization degree of the polyvinyl alcohol-based resin is preferably in the range of 1500 to 7000, and more preferably in the range of 2000 to 5000.
  • a polymerization degree of 1500 or more is preferable because crack resistance of the coating film during formation of the refractive index layer is improved.
  • the degree of polymerization is 7000 or less, the coating liquid at the time of forming the refractive index layer is preferable.
  • the semiconductor nanoparticles are formed by immersing the semiconductor nanoparticles in a solution containing the water-soluble resin under vacuum for a certain period of time. Can do.
  • thermoplastic resins such as a polymethylmethacrylate resin (PMMA; Poly (methyl methacrylate)
  • PMMA polymethylmethacrylate resin
  • a thermosetting resin such as a thermosetting urethane resin, a phenol resin, a urea melamine resin, an epoxy resin, an unsaturated polyester resin, or a silicone resin may be used.
  • the constituent semiconductor nanoparticle layer contains at least one compound selected from polysilazane and a modified polysilazane.
  • the polysilazane modified product is preferably a compound that is generated by subjecting polysilazane to a modification treatment and includes at least one selected from silicon oxide, silicon nitride, and silicon oxynitride.
  • the polysilazane may be dispersed together with the semiconductor nanoparticles in the coating solution for forming the semiconductor nanoparticle layer, or the semiconductor nanoparticles are coated with polysilazane in advance, and the particles are in the coating solution for forming the semiconductor nanoparticle layer. May be dispersed.
  • the term “covering” means covering the surface of the semiconductor nanoparticles, but the surface of the semiconductor nanoparticles may not cover all, but covers a part. It may be. Whether or not this condition is satisfied can be determined by analyzing the structure of the semiconductor nanoparticles coated with the resin by the above confirmation method.
  • the semiconductor nanoparticle layer is provided with durability capable of suppressing contact of the semiconductor nanoparticles with oxygen or the like over a long period of time. Furthermore, it can be set as a highly transparent layer.
  • Constituent material of polysilazane is a polymer having a silicon-nitrogen bond, and is composed of SiO 2 , Si 3 N 4 composed of Si—N, Si—H, NH, etc. Ceramic precursor inorganic polymer such as intermediate solid solution SiO x N y .
  • a polysilazane and a polysilazane derivative are compounds having a structure represented by the following general formula (I).
  • R 1 , R 2 and R 3 each independently represent a hydrogen atom, an alkyl group, an alkenyl group, a cycloalkyl group, an aryl group, an alkylsilyl group, an alkylamino group or an alkoxy group. .
  • PHPS Perhydropolysilazane
  • organopolysilazane in which part of the hydrogen part bonded to Si is substituted with an alkyl group or the like has an alkyl group such as a methyl group, so that the adhesion to the base material is improved and the polysilazane which is hard and brittle It is possible to impart toughness to the ceramic film by the above, and there is an advantage that generation of cracks can be suppressed even when the (average) film thickness is increased.
  • These perhydropolysilazane and organopolysilazane may be appropriately selected according to the application, and can also be mixed and used.
  • Perhydropolysilazane is presumed to have a linear structure and a ring structure centered on 6- and 8-membered rings. Its molecular weight is about 600 to 2000 (polystyrene conversion) in terms of number average molecular weight (Mn), is a liquid or solid substance, and varies depending on the molecular weight. These are commercially available in a solution state dissolved in an organic solvent, and the commercially available product can be used as it is as a polysilazane-containing liquid.
  • a silicon alkoxide-added polysilazane obtained by reacting the polysilazane represented by the general formula (I) with a silicon alkoxide (see, for example, JP-A No.
  • glycidol A glycidol-added polysilazane obtained by reacting see, for example, JP-A-6-122852
  • an alcohol-added polysilazane obtained by reacting an alcohol see, for example, JP-A-6-240208
  • a metal carboxylate Metal carboxylate-added polysilazane obtained by reaction for example, see JP-A-6-299118
  • acetylacetonate complex-added polysilazane obtained by reacting a metal-containing acetylacetonate complex for example, JP-A-6-299 No. 306329 Irradiation
  • fine metal particles of the metal particles added polysilazane obtained by adding e.g., JP-see JP 7-196986
  • amines and metal catalysts can be added to the semiconductor nanoparticle layer in order to promote the conversion of polysilazane into a silicon oxide compound.
  • Specific examples include Aquamica NAX120-20, NN110, NN310, NN320, NL110A, NL120A, NL150A, NP110, NP140, and SP140 manufactured by AZ Electronic Materials.
  • Modification treatment is preferably performed on the polysilazane contained in the semiconductor nanoparticle layer, whereby a part or all of the polysilazane contained in the semiconductor nanoparticle layer is modified by polysilazane modification. Become a body.
  • the modification treatment is performed on the coating layer formed by coating the coating solution for forming a semiconductor nanoparticle layer.
  • the modification treatment may be performed in advance on the semiconductor nanoparticles coated with the polysilazane, or may be coated with the polysilazane. It may be performed on the coating layer formed by coating the semiconductor nanoparticles, or may be performed on both.
  • a known method based on the conversion reaction of polysilazane can be selected.
  • Production of a silicon oxide film or a silicon oxynitride film by a substitution reaction of a silazane compound requires a heat treatment at 450 ° C. or more, and is difficult to apply to a flexible substrate such as plastic.
  • a method such as plasma treatment, ozone treatment, or ultraviolet irradiation treatment that allows the conversion reaction to proceed at a low temperature.
  • ultraviolet irradiation ultraviolet irradiation
  • vacuum ultraviolet irradiation excimer irradiation
  • plasma irradiation vacuum ultraviolet irradiation
  • VUV vacuum ultraviolet irradiation
  • UV irradiation treatment treatment by ultraviolet irradiation is also preferred.
  • Ozone and active oxygen atoms generated by ultraviolet light have high oxidation ability, and modify polysilazane at low temperature to produce silicon oxide or silicon oxynitride with high density and insulation. Is possible.
  • any commonly used ultraviolet ray generator can be used.
  • ultraviolet rays generally refers to electromagnetic waves having a wavelength in the range of 10 to 400 nm, but in the case of ultraviolet irradiation treatment in order to distinguish from the vacuum ultraviolet ray (10 to 200 nm) treatment described later. Preferably uses ultraviolet rays in the range of 210 to 350 nm.
  • UV irradiation For UV irradiation, set the irradiation intensity and irradiation time as long as the substrate carrying the applied coating film is not damaged.
  • Examples of the ultraviolet ray generation method used for the modification include a metal halide lamp, a high-pressure mercury lamp, a low-pressure mercury lamp, a xenon arc lamp, a carbon arc lamp, and an excimer lamp (single wavelengths of 172 nm, 222 nm, and 308 nm, for example, USHIO (Made by Co., Ltd.), UV light laser etc. are mentioned, It does not specifically limit.
  • a method of applying the ultraviolet rays from the generation source to the coating layer after reflecting the ultraviolet rays from the generation source is desirable in order to achieve uniform irradiation and improve efficiency. .
  • UV irradiation can be adapted to either batch processing or continuous processing, and can be appropriately selected depending on the shape of the substrate to be coated.
  • a more preferable modification treatment method is treatment by vacuum ultraviolet radiation.
  • the treatment by vacuum ultraviolet irradiation uses light energy in the range of 100 to 200 nm, preferably light energy having a wavelength in the range of 100 to 180 nm, which is larger than the interatomic bonding force in the silazane compound, and bonds the atoms.
  • This is a method of forming a silicon oxide film at a relatively low temperature by causing an oxidation reaction with active oxygen or ozone to proceed while cutting directly by the action of only photons called a photon process.
  • a rare gas excimer lamp is preferably used.
  • the detailed contents and specific conditions of the vacuum ultraviolet irradiation treatment are not particularly limited.
  • paragraphs [0079] to [0091] of JP 2011-031610 A The contents described therein or the contents described in paragraph numbers [0086] to [0098] of JP 2012-016854 A can be referred to.
  • the light-emitting device of the present invention includes an optical film containing the above-described semiconductor nanoparticles of the present invention.
  • FIG. 2 is a schematic cross-sectional view showing an example of the configuration of a light-emitting device provided with an optical film containing the semiconductor nanoparticles of the present invention.
  • the light emitting device 1 includes a blue or ultraviolet light source 3 (also referred to as a primary light source) and an image display panel 2 disposed in an optical path from the light source 3.
  • the image display panel 2 includes an image display layer 7 such as a liquid crystal layer.
  • Components such as a substrate for supporting the image display layer 7, electrodes and drive circuits for driving the image display layer, and an alignment film for aligning the liquid crystal layer in the case of the liquid crystal image display layer are shown in FIG. It is omitted in 2.
  • the image display layer 7 is a pixelated image display layer.
  • individual regions (“pixels”) of the image display layer are used as other regions. And can be driven independently.
  • the light-emitting device 1 of the present invention is intended to provide a color display. Therefore, the image display panel 2 is provided with a color filter unit 6.
  • the image display panel 2 includes a red color filter 6R, a blue color filter 6B, and a green color filter 6G, as shown in the figure.
  • a plurality of filter set units 6 are provided. The individual color filters are aligned with the pixels or sub-pixels of each image display layer 7 and installed.
  • the light source 3 may include one or more light emitting diodes (LEDs), and is preferably a blue light source or an ultraviolet light source.
  • LEDs light emitting diodes
  • the light emitting device 1 has a light guide 5 as an optical system that enables the image display panel 2 to be illuminated substantially uniformly by light from the light source 3.
  • the optical system includes a light guide 5 having a light emission surface 5 a that has substantially the same extent as the image display panel 2.
  • the light from the light source 3 enters the light guide 8 along the light incident surface 5b, is reflected in the light guide 5 according to the principle of total internal reflection, and finally the light emission surface 5a of the light guide. Radiated from.
  • the light guide body having such a configuration is publicly known, and details of the light guide body 5 are omitted here.
  • the optical film 4 of the present invention is provided on the emission surface 5 a of the light guide 5.
  • the optical film 4 containing the semiconductor nanoparticles of the present invention emits light in a plurality of wavelength ranges different from each other and different from the emission wavelength range of the primary light source 3 when illuminated by light from the primary light source 3. It is preferably composed of two or more different materials.
  • the primary light source 3 preferably emits light outside the visible spectrum region (for example, light in the ultraviolet (UV) region) or blue light.
  • the color filter unit 6 shown in FIG. 2 includes a color filter having a narrow transmission band.
  • the narrow transmission band filter preferably has a full width at half maximum (FWHM) of 100 nm or less, and particularly preferably has a FWHM of 80 nm or less.
  • an optical film 4 may be provided inside the light guide 5 main body.
  • the semiconductor nanoparticles according to the present invention are disposed in a suitable transparent matrix, for example, in a resin that is molded to have a desired shape of the light guide 5 and then curved. It can be set as the optical film 4 comprised.
  • Example 1 ⁇ Synthesis of semiconductor nanoparticles> [Synthesis of Semiconductor Nanoparticle A: Core / Shell InP / ZnS Semiconductor Nanoparticle A] Indium myristate 0.1 mmol, stearic acid 0.1 mmol, trimethylsilylphosphine 0.1 mmol, dodecanethiol 0.1 mmol, and undecylenic acid zinc 0.1 mmol were placed in a three-necked flask together with octadecene 8 ml and refluxed under a nitrogen atmosphere. The mixture was heated at 0 ° C.
  • the semiconductor nanoparticle A having a core / shell structure is represented by InP / ZnS, where the core is InP and the shell is ZnS.
  • the semiconductor nanoparticle A was directly observed with a transmission electron microscope, and it was confirmed that the surface of the InP core part was an InP / ZnS semiconductor nanoparticle having a core / shell structure coated with a ZnS shell. Further, according to this observation, the InP / ZnS semiconductor nanoparticles A synthesized by this synthesis method have a core part particle diameter in the range of 2.1 to 3.8 nm and a core part particle size distribution of 6 to 40. %.
  • a JEM-2100 transmission electron microscope manufactured by JEOL Ltd. was used for the observation.
  • the optical properties of the InP / ZnS semiconductor nanoparticles A were measured using an octadecene solution containing the semiconductor nanoparticles A. It was confirmed that the emission peak wavelength was in the range of 430 to 720 nm, and the emission half width was in the range of 35 to 90 nm. The luminous efficiency reached a maximum of 70.9%.
  • a fluorescence spectrophotometer FluoroMax-4 manufactured by JOBIN YVON is used to measure the emission characteristics of InP / ZnS semiconductor nanoparticles A, and a spectrophotometer manufactured by Hitachi High-Technologies Corporation is used to measure the absorption spectrum. A total of U-4100 was used.
  • TOPO trioctylphosphine oxide
  • HDA 1-heptadecyl-octadecylamine
  • the synthesized semiconductor nanoparticle B is directly observed with a transmission electron microscope, whereby a CdSe / ZnS semiconductor nanoparticle having a core / shell structure in which the surface of the CdSe core is covered with a ZnS shell. I was able to confirm that. In addition, it was confirmed that the CdSe / ZnS semiconductor nanoparticles B had a core part particle size in the range of 2.0 to 4.0 nm and a core part particle size distribution in the range of 6 to 40%. As for the optical characteristics, it was confirmed that the emission peak wavelength was in the range of 410 to 700 nm and the emission half width was in the range of 35 to 90 nm. The luminous efficiency reached a maximum of 73.9%.
  • the synthesized core / shell structure InP / ZnS semiconductor nanoparticles A were dispersed in 0.5 ml of chloroform, and then filtered to remove insoluble matters.
  • the semiconductor nanoparticle A-chloroform dispersion was added to the microspheres dispersed in toluene prepared above, and shaken on a shaker plate at room temperature for 16 hours for thorough mixing.
  • the semiconductor nanoparticles A-microspheres were centrifuged and settled, and the supernatant liquid containing excess semiconductor nanoparticles A was drained.
  • the precipitate was washed twice with 2 ml of toluene, and the washed precipitate was resuspended in toluene (2 ml) and then transferred to a glass sample Bayer tube.
  • TMPTM which is a crosslinking agent was added to the liquid mixture of MMA and the semiconductor nanoparticle C, and the mixture of the monomer and the crosslinking agent was stirred with a whirl mixer.
  • the prepared slurry was transferred to a syringe, and then continuously stirred at 1200 rpm while being poured into 5 ml of 2% polyvinyl acetate (abbreviation: PVAc) deaerated from the syringe.
  • PVAc polyvinyl acetate
  • cyclohexane / CO-520 see below
  • the obtained particles were washed twice with 20 ml of cyclohexane and dried under vacuum to obtain a powder of InP / ZnS semiconductor nanoparticles K having a core / shell structure in which silica was coated on the particle surfaces.
  • CO-520 Igepal (registered trademark) CO-520 (nonionic surfactant), polyoxyethylene (5) nonylphenyl ether [4- (C 9 H 19 ) C 6 H 4 O (CH 2 CH 2 O) 4 CH 2 CH 2 OH]
  • Preparation of semiconductor nanoparticle L Preparation of Semiconductor Nanoparticle L with InP Structure Coated with UV-Curable Resin 1
  • semiconductor nanoparticles L 1 having an InP structure were prepared by the following method.
  • Dibutyl ester (100 ml) and myristic acid (10.0627 g) were placed in a three-necked flask and degassed at 70 ° C. under vacuum for 1 hour. Nitrogen gas was then introduced and the temperature was raised to 90 ° C. ZnS molecular cluster [Et 3 NH 4 ] [Zn 10 S 4 (SPh) 16 ] (4.77076 g) was added and the mixture was stirred for 45 minutes. Then, after raising the temperature to 100 ° C., In (MA) 3 (1 mol / L, 15 ml) was added dropwise (TMS) 3 P (1 mol / L, 15 ml). The temperature was raised to 140 ° C. while stirring the reaction mixture.
  • degassed dry methanol (about 200 ml) was added to separate the nanoparticles. After allowing the precipitate to settle, the methanol was removed via a cannula with the help of a filter rod. Degassed dry chloroform (about 10 ml) was added to wash the solids. The solid was dried under vacuum for 1 day. Thereby, 5.60 g of semiconductor nanoparticles L 1 having an InP structure were prepared.
  • the InP semiconductor nanoparticles L 1 prepared as described above were washed with dilute hydrofluoric acid (HF) acid.
  • Semiconductor nanoparticles L were dissolved in degassed anhydrous chloroform ( ⁇ 270 ml). A 50 ml portion was removed and placed in a plastic flask and flushed with nitrogen. Using a plastic syringe, 3 ml of 60 wt / wt% HF was added to water and added to degassed tetrahydrofuran (THF) (17 ml) to make an HF solution. HF was added dropwise to the semiconductor nanoparticles L over 5 hours. After the addition was complete, the solution was left stirring overnight. Excess HF was removed by drying the etched InP semiconductor nanoparticles L 1 through extraction with an aqueous calcium chloride solution.
  • HF degassed tetrahydrofuran
  • HDA 500 g was placed in a three-necked round bottom flask and heated to 120 ° C. for 1 hour or more under dynamic vacuum to dry and degas. The solution was then cooled to 60 ° C. To this was added 0.718 g of [HNEt 3 ] 4 [Cd 10 Se 4 (SPh) 16 ] (0.20 mmol). In total, 42 mmol, 22.0 ml of TOPSe, and 42 mmol (19.5 ml, 2.15 M) of Me 2 Cd ⁇ TOP were used. First, 4 mmol of TOPSe and 4 mmol of Me 2 Cd ⁇ TOP were added to the reaction solution at room temperature, and the temperature was raised to 110 ° C. and stirred for 2 hours.
  • the reaction solution was dark yellow, and the temperature was gradually raised at a rate of ⁇ 1 ° C./5 min while adding equimolar amounts of TOPSe and Me 2 Cd ⁇ TOP dropwise.
  • the reaction was stopped by cooling to 60 ° C. and then adding 300 ml of dry ethanol or acetone. This produced a deep red particle precipitate that was further separated by filtration.
  • the resulting CdSe particles were redissolved in toluene and then filtered through celite followed by recrystallization from warm ethanol to remove any excess HDA, selenium or cadmium present. This produced 10.10 g of CdSe semiconductor nanoparticles M 1 capped with HDA.
  • optical films 1 to 22 were produced by the following method.
  • coating of the coating liquid were performed in the environment which interrupted
  • the above-mentioned coating solution 1 for forming a semiconductor nanoparticle layer has a dry film thickness of 100 ⁇ m on a 125 ⁇ m-thick polyethylene terephthalate film (KDL86WA, abbreviated as PET: manufactured by Teijin DuPont Films, Ltd.) with easy adhesion processing on both sides. It apply
  • KDL86WA polyethylene terephthalate film
  • Excimer lamp light intensity 130 mW / cm 2 (172 nm)
  • Distance between sample and light source 1mm
  • Stage heating temperature 70 ° C
  • Oxygen concentration in the irradiation device 0.01%
  • Excimer lamp irradiation time 5 seconds.
  • Optical films 2 to 6 of the present invention were produced in the same manner as the production of the optical film 1 except that the semiconductor nanoparticles E were changed to the respective semiconductor nanoparticles shown in Table 1.
  • optical films 7 and 8 were prepared in the same manner as the optical film 1 except that the semiconductor nanoparticles E were changed to the semiconductor nanoparticles shown in Table 1 and no excimer irradiation was performed.
  • Optical films 9 to 11 of comparative examples were produced in the same manner as in the production of the optical film 1 except that the semiconductor nanoparticles E were changed to the respective semiconductor nanoparticles shown in Table 1.
  • the semiconductor nanoparticle layer forming coating solution 12 was applied to a 125 ⁇ m-thick polyethylene terephthalate film (KDL86WA, manufactured by Teijin DuPont Films, Ltd.) with easy adhesion on both sides so that the dry film thickness was 100 ⁇ m.
  • the film was dried at 3 ° C. for 3 minutes and cured under a curing condition: 0.5 J / cm 2 air using a high-pressure mercury lamp to produce an optical film 12 of a comparative example.
  • Optical films 13 to 16 of comparative examples were produced in the same manner as the production of the optical film 12 except that the semiconductor nanoparticles E were changed to the respective semiconductor nanoparticles shown in Table 1.
  • optical film 17 of the present invention was prepared in the same manner as the optical film 5 except that the substrate was changed to a polycarbonate film having a thickness of 100 ⁇ m (manufactured by Teijin Chemicals Ltd., Pure Ace WR-S5, abbreviated as PC). .
  • optical film 18 was produced in the same manner as the production of the optical film 5 except that the substrate was changed to a triacetyl cellulose film having a thickness of 100 ⁇ m (manufactured by Konica Minolta, abbreviation: TAC).
  • optical film 19 of the present invention was produced in the same manner as the production of the optical film 5 except that the base material was changed to a cycloolefin polymer film having a thickness of 100 ⁇ m (manufactured by Nippon Zeon Co., Ltd., abbreviation: COP).
  • the particle size was adjusted so that the semiconductor nanoparticles E emitted red and green light.
  • PHPS perhydropolysilazane
  • PHPS Aquamica NN120-10, manufactured by non-catalytic type, AZ Electronic Materials Co.
  • a 4.12mg of semiconductor nanoparticles E G green light is dispersed in toluene solvent, by adding further perhydropolysilazane (PHPS, Aquamica NN120-10, manufactured by non-catalytic type, AZ Electronic Materials Co.)
  • PHPS perhydropolysilazane
  • a coating solution G for forming a green semiconductor nanoparticle layer in which the mass content of the semiconductor nanoparticles was 1.0% was prepared.
  • the prepared red light emitting semiconductor nanoparticle layer forming coating solution R is applied to a 125 ⁇ m thick polyethylene terephthalate film (KDL86WA, manufactured by Teijin DuPont Films, Ltd.) with easy adhesion on both sides, and the dry film thickness is 100 ⁇ m.
  • the coating was carried out under the following conditions and dried at 60 ° C. for 3 minutes.
  • excimer irradiation was performed with the following excimer apparatus.
  • the green light emitting semiconductor nanoparticle layer forming coating solution G was applied on the red light emitting semiconductor nanoparticle layer R under the condition that the dry film thickness was 100 ⁇ m, and dried at 60 ° C. for 3 minutes.
  • excimer irradiation was performed with the following excimer apparatus to produce an optical film 20 of the present invention having a semiconductor nanoparticle layer having a two-layer structure of red light emission / green light emission.
  • optical film 21 was prepared in the same manner as the optical film 3 except that the semiconductor nanoparticles G were changed to the semiconductor nanoparticles L shown in Table 1.
  • optical film 22 was prepared in the same manner as the optical film 4 except that the semiconductor nanoparticles H were changed to the semiconductor nanoparticles M shown in Table 1.
  • PET Polyethylene terephthalate film
  • PC Polycarbonate film
  • TAC Triacetylcellulose film
  • COP Cycloolefin polymer film (Coating material for semiconductor nanoparticles)
  • PVA Polyvinyl alcohol (water-soluble resin)
  • PMMA Polymethylmethacrylate (acrylic resin)
  • PMMA Polylauryl methacrylate (acrylic resin) (Dispersion retention material)
  • PHPS Perhydropolysilazane
  • UV polymer UV curable resin (Modification after coating)
  • VUV Vacuum ultraviolet irradiation (excimer irradiation)
  • UV UV irradiation (high pressure mercury lamp)
  • the optical film is preferably less than 1.5% ( ⁇ to ⁇ ⁇ ) from the viewpoint of use in a light emitting device.
  • Relative luminous efficiency is 125 or more.
  • Each optical film produced was subjected to an accelerated deterioration treatment for 3000 hours in an environment of 85 ° C. and 85% RH, and then the light emission efficiency was measured by the same method as the evaluation of the light emission characteristics.
  • the ratio of the luminous efficiency after the accelerated deterioration process to the luminous efficiency was determined, and the durability was evaluated according to the following criteria.
  • ⁇ The value of the luminous efficiency ratio before and after the accelerated deterioration treatment is 0.95 or more.
  • ⁇ ⁇ The value of the luminous efficiency ratio before and after the accelerated deterioration treatment is 0.90 or more and less than 0.95.
  • ⁇ The ratio value of the luminous efficiency before and after the accelerated deterioration process is 0.80 or more and less than 0.90.
  • ⁇ ⁇ The ratio value of the luminous efficiency before and after the accelerated deterioration process is 0.50 or more, 0. Less than .80 ⁇ : The value of the ratio of the luminous efficiency before and after the accelerated deterioration treatment is less than 0.50.
  • Table 1 shows the evaluation results obtained as described above.
  • the optical film of the present invention is higher in transparency and superior in luminous efficiency and durability than the comparative example.
  • Example 2 ⁇ Production of light emitting device>
  • the optical films 1 to 22 produced in Example 1 were provided in the light emitting device shown in FIG. 2 to produce the light emitting devices 1 to 22.
  • each optical film 4 was pasted on the light emitting surface 5 a of the light guide 5.
  • the optical film of the present invention is excellent in luminous efficiency and has excellent durability capable of suppressing deterioration of semiconductor nanoparticles due to oxygen or the like over a long period of time, and high transparency. It can be suitably used as an optical film for various light emitting devices such as space illumination and electroluminescent displays.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Nonlinear Science (AREA)
  • Mathematical Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Optical Filters (AREA)
  • Laminated Bodies (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Luminescent Compositions (AREA)
  • Led Device Packages (AREA)

Abstract

L'objectif de la présente invention est de fournir: un film optique qui a une transparence excellent et est doté d'une durabilité qui permet la suppression de la détérioration des nanoparticules semi-conductrices pendant une longue période de temps, ladite détérioration étant provoquée par l'oxygène ou similaire; et un dispositif d'émission de lumière qui est fourni avec ce film optique. Un film optique selon la présente invention comprend une base et une couche de nanoparticules semi-conductrices qui est présente sur la base. Ce film optique est caractérisé en ce que la couche de nanoparticules semi-conductrices contient des nanoparticules semi-conductrices, chacunes desquelles étant recouverte par une résine, et un polysilazane ou un polysilazane modifié, dans lesquels les nanoparticules semi-conductrices sont dispersées et retenues.
PCT/JP2014/065688 2013-06-25 2014-06-13 Film optique et dispositif d'émission de lumière WO2014208356A1 (fr)

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JP2016167041A (ja) * 2015-03-03 2016-09-15 大日本印刷株式会社 高演色液晶表示装置およびカラーフィルタ
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JP2017534894A (ja) * 2014-08-14 2017-11-24 エルジー・ケム・リミテッド 発光フィルム（ｌｉｇｈｔ−ｅｍｉｔｔｉｎｇ ｆｉｌｍ）
JP2018506625A (ja) * 2015-12-23 2018-03-08 アファンタマ アクチェンゲゼルシャフト 発光部品
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WO2018114761A1 (fr) 2016-12-20 2018-06-28 Merck Patent Gmbh Milieu optique et dispositif optique
WO2018116882A1 (fr) * 2016-12-19 2018-06-28 富士フイルム株式会社 Film de conversion de longueur d'onde et procédé de production d'un film de conversion de longueur d'onde
JP2018106097A (ja) * 2016-12-28 2018-07-05 大日本印刷株式会社 光波長変換部材、バックライト装置、および画像表示装置
WO2018212268A1 (fr) * 2017-05-17 2018-11-22 住友化学株式会社 Film ainsi que procédé de fabrication de celui-ci, procédé de fabrication de composition, et procédé de fabrication d'article durci
JP2019502955A (ja) * 2015-12-23 2019-01-31 アファンタマ アクチェンゲゼルシャフト ルミネセント構成部品
JP2019506510A (ja) * 2016-02-12 2019-03-07 ナノコ テクノロジーズ リミテッド 安定性に優れた量子ドット含有ポリマーフィルム
CN109661598A (zh) * 2016-09-02 2019-04-19 富士胶片株式会社 含荧光体薄膜及背光单元
WO2022036511A1 (fr) * 2020-08-17 2022-02-24 深圳市汇顶科技股份有限公司 Filtre optique passe-bande infrarouge et système de capteur

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JP2019506510A (ja) * 2016-02-12 2019-03-07 ナノコ テクノロジーズ リミテッド 安定性に優れた量子ドット含有ポリマーフィルム
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WO2017167779A1 (fr) 2016-03-31 2017-10-05 Merck Patent Gmbh Feuille de conversion de couleurs et dispositif optique
CN109661598A (zh) * 2016-09-02 2019-04-19 富士胶片株式会社 含荧光体薄膜及背光单元
JP2020181196A (ja) * 2016-11-16 2020-11-05 Ｎｓマテリアルズ株式会社 量子ドット含有部材、シート部材、バックライト装置、及び、表示装置
WO2018092705A1 (fr) * 2016-11-16 2018-05-24 Ｎｓマテリアルズ株式会社 Élément contenant des points quantiques, élément feuille, dispositif de rétroéclairage et dispositif d'affichage
CN110268287A (zh) * 2016-11-16 2019-09-20 Ns材料株式会社 含量子点的部件、薄片部件、背光装置及显示装置
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JP2018101000A (ja) * 2016-12-19 2018-06-28 富士フイルム株式会社 波長変換フィルムおよび波長変換フィルムの製造方法
WO2018116882A1 (fr) * 2016-12-19 2018-06-28 富士フイルム株式会社 Film de conversion de longueur d'onde et procédé de production d'un film de conversion de longueur d'onde
WO2018114761A1 (fr) 2016-12-20 2018-06-28 Merck Patent Gmbh Milieu optique et dispositif optique
JP2018106097A (ja) * 2016-12-28 2018-07-05 大日本印刷株式会社 光波長変換部材、バックライト装置、および画像表示装置
CN110621745A (zh) * 2017-05-17 2019-12-27 住友化学株式会社 薄膜、组合物的制造方法、固化物的制造方法及薄膜的制造方法
WO2018212268A1 (fr) * 2017-05-17 2018-11-22 住友化学株式会社 Film ainsi que procédé de fabrication de celui-ci, procédé de fabrication de composition, et procédé de fabrication d'article durci
CN110621745B (zh) * 2017-05-17 2022-03-29 住友化学株式会社 薄膜、组合物的制造方法、固化物的制造方法及薄膜的制造方法
WO2022036511A1 (fr) * 2020-08-17 2022-02-24 深圳市汇顶科技股份有限公司 Filtre optique passe-bande infrarouge et système de capteur

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