WO2014038332A1 - 高速応答性フォトリフラクティブポリマー素子 - Google Patents
高速応答性フォトリフラクティブポリマー素子 Download PDFInfo
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- WO2014038332A1 WO2014038332A1 PCT/JP2013/071190 JP2013071190W WO2014038332A1 WO 2014038332 A1 WO2014038332 A1 WO 2014038332A1 JP 2013071190 W JP2013071190 W JP 2013071190W WO 2014038332 A1 WO2014038332 A1 WO 2014038332A1
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- 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
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- G02B27/4205—Diffraction optics, i.e. systems including a diffractive element being designed for providing a diffractive effect having a diffractive optical element [DOE] contributing to image formation, e.g. whereby modulation transfer function MTF or optical aberrations are relevant
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- 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
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- 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
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- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
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- 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
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- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
- G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
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- G03H2001/0264—Organic recording material
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- G—PHYSICS
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- G03H2260/00—Recording materials or recording processes
- G03H2260/50—Reactivity or recording processes
- G03H2260/54—Photorefractive reactivity wherein light induces photo-generation, redistribution and trapping of charges then a modification of refractive index, e.g. photorefractive polymer
Definitions
- the present invention relates to a photorefractive polymer element, and more particularly to a high-speed responsive photorefractive polymer element using a triphenylamine polymer as a host polymer.
- the photorefractive effect is one of nonlinear optical effects, and is a phenomenon in which a substance absorbs light and its refractive index changes.
- the mechanism of expression of the photorefractive effect will be described.
- This spatial electric field causes a Pockels effect which is a first-order electro-optic effect, and a periodic refractive index grating is formed. Since a phase difference of ⁇ occurs spatially between the refractive index grating and the optical interference paper, asymmetric energy transfer is observed between the two light waves, and optical amplification (optical gain) is obtained.
- nonlinear optical information including phase conjugation, imaging from distorted media, real-time holography, super-multiplex hologram recording, 3D display, 3D printer, optical amplification, and optical neutral network
- processing, pattern recognition, optical limiting, storage of high-density optical data, and the like are expected.
- an inorganic crystal material such as lithium niobate (LiNbO3) has been used as a photorefractive material that exhibits the above effects.
- this inorganic crystal material has a problem of poor workability.
- development of photorefractive materials made of organic substances has been active.
- Organic photorefractive materials have many advantages over inorganic photorefractive materials. Advantages include easy optimization of the composition ratio and high workability, as well as large optical nonlinearity, low dielectric constant, low cost, light weight, flexibility, and the like. Other important characteristics that may be desirable depending on the application include long shelf life of recorded data, optical quality, and thermal stability. Such organic photorefractive materials are becoming important materials for advanced information communication technology. Among these, carbazoles (see, for example, Patent Document 1) and triphenylamines are known.
- Patent Document 2 describes a photorefractive element in which a layer containing a photorefractive material and a layer containing an electron / ion mixed conductor are sandwiched between two transparent electrode substrates.
- the photorefractive material constituting the photorefractive element of Patent Document 2 is made of an inorganic crystal material such as lithium niobate or a polymer material, and the electron / ion mixed conductor is made of silver sulfide.
- an inorganic crystal material such as lithium niobate or a polymer material
- the electron / ion mixed conductor is made of silver sulfide.
- an object of the present invention is to provide a high-speed responsive photorefractive polymer element with significantly improved responsiveness.
- the present inventors have intensively studied to solve the above problems. In order to improve responsiveness, it is important to select a compound that provides high responsiveness for constructing a photorefractive polymer element, and to suppress the generation of dark current associated with the selection of this compound. Pay attention. As a result, the inventors have found that the above-described problems can be solved by selecting a triphenylamine polymer as a photorefractive polymer and further including a self-assembled monomolecular film in the constitution, and the present invention has been completed.
- the fast response photorefractive polymer element of the present invention includes an insulating substrate, a transparent electrode formed on one surface of the insulating substrate, a dark current control layer formed on the surface of the transparent electrode, and the insulating substrate.
- the photorefractive composite material provided through the transparent electrode and the dark current control layer is provided.
- the fast responsive photorefractive polymer element of the present invention includes another insulating substrate disposed substantially parallel to the insulating substrate, another transparent electrode formed on the inner surface of the other insulating substrate, Another dark current control layer formed on the inner surface of another transparent electrode, and the photorefractive composite material is interposed between the pair of insulating substrates via the transparent electrode and the dark current control layer. It is characterized by being pinched.
- the dark current control layer formed on the surface of the transparent electrode and the photorefractive composite material provided on the insulating substrate via the transparent electrode and the dark current control layer.
- Generation of dark current can be suppressed by the dark current control layer while exhibiting high responsiveness by the composite material.
- a photorefractive polymer element with significantly improved responsiveness can be obtained.
- the dark current control layer is not limited, but is preferably a single-layer monomolecular film or a plurality of monolayers formed on the surface of the transparent electrode.
- the Fermi potential of the transparent electrode is made shallow by providing a monolayer or monolayer of a single layer between the transparent electrode and the photorefractive composite material, for example, generation of dark current due to the selection of the photorefractive polymer. Can be efficiently suppressed.
- the monolayer monolayer or monolayer monolayer is not limited, but is preferably formed by chemically modifying a silane compound on the surface of the transparent electrode.
- the silane compound is not limited, but 3-aminopropyltrimethoxysilane is preferable. By selecting 3-aminopropyltrimethoxysilane as the silane compound, the generation of dark current can be minimized.
- the single-layer monomolecular film or the multi-layer monolayer can be formed by various methods.
- the monomolecular film is obtained by chemically modifying 3-aminopropyltrimethoxysilane, it is preferably formed by the following method. That is, the transparent electrode substrate on which the transparent electrode is formed on the insulating substrate is hydrophilized by immersing it in a mixed solution of ammonia water and hydrogen peroxide or in a piranha solution.
- an integrated precursor is produced by immersion in a mixed solvent of aminopropyltrimethoxysilane, and the surface of the integrated precursor is washed with alcohol to remove excess molecules.
- a single-layer monomolecular film or a multi-layer monomolecular film is formed using the above method, ordered monolayers can be obtained, and the effect of suppressing dark current can be improved.
- the thickness is preferably equal to or more than one molecule of the silane compound in order to obtain a high dark current suppressing effect.
- the photorefractive composite material preferably contains a photorefractive polymer represented by the following formula (1).
- the photorefractive composite material further includes a nonlinear optical dye, a sensitizer, and a plasticizer.
- the photorefractive polymer is contained in 10 to 50% by weight
- the nonlinear optical dye is contained in 20 to 50% by weight
- the sensitizer is contained in 0.1 to 3% by weight
- the plasticizer is contained in 10 to 40% by weight.
- it is.
- a dark current control layer formed on the surface of the transparent electrode and a photorefractive composite material provided on the insulating substrate via the transparent electrode and the dark current control layer are provided.
- the dark current control layer can suppress the generation of dark current while exhibiting high responsiveness by the photorefractive polymer. As a result, a photorefractive polymer element with significantly improved responsiveness can be obtained.
- FIG. 1 is a schematic cross-sectional view of a fast responsive photorefractive polymer element according to an embodiment of the present invention. It is a figure for demonstrating the problem in the case of selecting PTAA as a photorefractive composite material. It is a figure for demonstrating the method of solving the problem in the case of selecting PTAA as a photorefractive composite material. It is a conceptual diagram at the time of forming a self-assembled monomolecular film on an ITO electrode substrate. It is the schematic for demonstrating the four-wave mixing method for measuring diffraction efficiency.
- 3 is a graph showing the relationship between the electric field strength and diffraction efficiency of Example 1.
- 3 is a graph showing time response of diffraction efficiency of Example 1.
- FIG. 1 is a schematic cross-sectional view of a fast responsive photorefractive polymer element 1 (hereinafter referred to as a photorefractive polymer element) according to an embodiment of the present invention.
- the photorefractive polymer element 1 of the present embodiment is formed on a pair of insulating substrates 2 and 2 arranged substantially parallel to each other as shown in FIG. 1 and on the inner surfaces 2a and 2a of the pair of insulating substrates 2 and 2, respectively.
- the photorefractive composite material 5 is interposed between the photorefractive composite material 5 and a spacer 6 provided around the photorefractive composite material 5.
- each layer is shown thicker than actual for description.
- Each insulating substrate 2 and each transparent electrode 3 formed on the inner surface 2a of each insulating substrate 2 constitute a pair of transparent electrode substrates 7 and 7 arranged in parallel to each other.
- the insulating substrate 2 is not limited, and specific examples of the insulating substrate 2 include, for example, soda lime glass, silica glass, borosilicate glass, gallium nitride, gallium arsenide, sapphire, quartz glass, polyethylene terephthalate, and polycarbonate.
- a composite substrate appropriately combined can be used.
- Each transparent electrode 3 formed on the inner surface 2a of each insulating substrate 2 is a conductive film, and can be selected from a metal oxide film, a metal film, an organic film, and the like.
- indium tin oxide (ITO) is selected as the transparent electrode 3 and configured as an ITO electrode, but is not limited thereto.
- Other specific examples of the transparent electrode 3 include tin oxide, zinc oxide, polythiophene, gold, silver, platinum, copper, aluminum, polyaniline, lithium, magnesium, magnesium-silver mixture, magnesium-indium mixture, aluminum-lithium alloy, carbon What consists of carbon, such as nanofiber, and those combination is mentioned.
- the photorefractive composite material 5 of the present embodiment can be obtained by adding a sensitizer, a nonlinear optical dye, and a plasticizer to the photorefractive polymer that is a main component.
- a sensitizer e.g., a nonlinear optical dye
- a plasticizer e.g., a plasticizer
- very high diffraction efficiency and gain coefficient can be obtained.
- charge transport in a stable and uniform film can be efficiently used, and a very high degree of photorefractive effect that cannot be achieved conventionally can be obtained.
- the sensitizer has performance as an electron acceptor and is blended in order to enhance photorefractive properties.
- a sensitizer is blended, a charge transfer complex is formed by the sensitizer and the photorefractive polymer, and useful photorefractive properties are expressed.
- [6,6] -phenyl C 61 butanoic acid methyl ester (PCBM) represented by the following formula (2) is used as a sensitizer.
- sensitizer examples include (2,4,7-trinitro-9-flurenylidene) malonitrile (TNF-DM), 2,4,7-trinitro-9-fluorenone (TNF), fullerene C 60 , fullerene.
- TCBN tetracyanobenzene
- TCNQ tetracyanoquinodinomethane
- BQ benzoquinone
- MQ 2,6-dimethyl-p-benzoquinone
- Cl 2 Q 2,5-dichloro-p-benzoquinone
- chloranil 2,3,5,6-tetrachloro-p-benzoquinone
- DDQ 2,3-dichloro-5,6-p-benzoquinone
- DDQ 2,3-dichloro-5,6-p-benzoquinone
- a sensitizer may be used individually by 1 type and may use 2 or more types together.
- the content of the sensitizer is preferably 0.1% by weight and more preferably 0.3% by weight as a lower limit with respect to 100% by weight of the photorefractive composite material.
- the upper limit is preferably 3% by weight, more preferably 1% by weight, and most preferably 0.6% by weight.
- the optimum content of the sensitizer is about 0.5% by weight.
- the content of the sensitizer is 0.1% by weight or less, the photorefractive property is lowered.
- the concentration of the charge transfer complex due to the sensitizer is increased, leading to an increase in light absorption and a significant decrease in light transmittance.
- the nonlinear optical dye is a donor-acceptor type molecule exhibiting second-order nonlinear optical characteristics, that is, a material whose refractive index changes with an electric field (second-order nonlinear optical material).
- second-order nonlinear optical material a material whose refractive index changes with an electric field.
- [[4- (hexahydro-1H-azepin-1-yl) phenyl] methylene] propanedinitrile (7-DCST) represented by the following formula (3) is used as the nonlinear optical dye.
- PDCST 4-piperidinobenzylidene-malononitrile
- 2- (4- (azepan-1-yl) represented by the following formula (5)
- FDCST -Fluoro-benzylidene
- nonlinear optical dyes include 2,5-dimethyl-4- (p-nitrophenylazo) anisole (DMNPAA), 4-amino-4′-nitroazobenzene (ANAB), s-( ⁇ )-1 -(4-nitrophenyl) -2-pyrrolidine-methanol (NPP), 4- (diethylamino)-(E) - ⁇ -nitrostyrene (DEANST), (diethylamino) benzaldehyde diphenylhydrazone (DEH), AODCST, TDDCST, And aminocyanostyrenes such as DCDHF-6.
- dye may be used individually by 1 type, and may use 2 or more types together.
- the content of the nonlinear optical dye is preferably 20% by weight, more preferably 25% by weight, more preferably 50% by weight, and preferably 40% by weight as the lower limit with respect to 100% by weight of the photorefractive composite material. % Is more preferable, and 30% by weight is most preferable. If the content of the nonlinear optical dye is less than 20% by weight, the diffraction efficiency and gain coefficient necessary for the photorefractive effect may not be obtained. If the content of the nonlinear optical dye is more than 50% by weight, an imbalance in the amount ratio with other components may occur, which may adversely affect the design of the photorefractive composite.
- the plasticizer serves to lower the glass transition temperature of the matrix.
- ethyl carbazole (ECz) represented by the following formula (6) is used as a sensitizer.
- plasticizer is (2,4,6-trimethylphenyl) diphenylamine (TAA) represented by the following formula (7).
- plasticizers include carbazoyl ethyl propionate (CzEPA), triphenylamine (TPA), benzyl butyl phthalate (BBP), dicyclohexyl phthalate (DCP) tricresyl phosphate (TCP), diphenyl phthalate ( DPP), N -methyl- 1 -pyrrolidone, N -octyl- 1 -pyrrolidone, N--alkyl- 1 -pyrrolidones such as N-dodecyl-1-pyrrolidone, and 2-(1,2-cyclohexanedicarboximide) Ethyl propionate (AX22), 2- (1,2-cyclohexanedicarboximido) ethyl butyrate, 2- (1,2-cyclohexanedicarboximido) ethyl benzoate, 2- (1,2-cyclohexanedicarboximide) ) Ethyl propionate
- the content of the plasticizer is preferably 10% by weight, more preferably 15% by weight, and more preferably 40% by weight, and 30% by weight as the lower limit with respect to 100% by weight of the photorefractive composite material. Is more preferred, with 20% by weight being most preferred. If the plasticizer content is less than 10% by weight, the glass transition temperature of the photorefractive polymer does not decrease, and the diffraction efficiency and gain coefficient required for the photorefractive effect may not be obtained. When the content of the plasticizer is more than 40% by weight, an unbalance is generated in the amount ratio with other components, which may adversely affect the design of the photorefractive composite.
- the photorefractive polymer is not limited, but is a triarylamine-based amorphous polymer polytriarylamine (PTAA) represented by the following formula (1) used in this embodiment: Poly [bis (4-phenyl) (2 , 4,6-trimethylphenyl) amine]. This is also called polytriarylamine semiconductors.
- PTAA triarylamine-based amorphous polymer polytriarylamine
- Poly [bis (4-phenyl) (2,4,6-trimethylphenyl) amine] is an amorphous P-type semiconductor with high carrier mobility.
- the mobility is 10 ⁇ 2 to 10 ⁇ 3 cm 2 / Vs, and when used in the photorefractive polymer element 1, very high responsiveness can be exhibited.
- a photorefractive polymer having a tetraphenyldiaminobiphenyl moiety also exhibits high responsiveness.
- the content of the photorefractive polymer represented by the above formula (1) is preferably 10% by weight, more preferably 20% by weight, and more preferably 30% by weight with respect to 100% by weight of the photorefractive composite material.
- the upper limit is preferably 50% by weight, and more preferably 40% by weight.
- the content is less than 10% by weight, the glass transition point may not be sufficiently lowered.
- other components may adversely affect the design of the photorefractive composite material.
- the thickness of the photorefractive composite material 5 is preferably 50 to 100 ⁇ m. If the thickness is less than 50 ⁇ m, it is difficult to satisfy the Bragg diffraction condition, and if it exceeds 100 ⁇ m, the applied voltage may increase or the absorption may increase. .
- the spacer 6 is not limited as long as it can maintain the thickness of the photorefractive composite material.
- a fluorine resin such as polyimide, PTFE, or PFA is preferable from the viewpoint of chemical resistance and heat resistance.
- Each dark current control layer 4 of the present embodiment is formed on the inner surface 7a of each transparent electrode substrate 7 (ITO electrode substrate) and covers the inner surface 7a. Therefore, each dark current control layer 4 is interposed between each transparent electrode substrate 7 and the photorefractive composite material 5, and each transparent electrode 3 and the photorefractive composite material 5 are not in contact with each other. .
- the dark current control layer 4 is preferably formed on both of the transparent electrode substrates 7, but may be formed only on one of the transparent electrode substrates depending on the performance to be exhibited.
- FIG. 2 is a diagram for explaining a problem when PTAA is selected as the photorefractive composite material 5
- FIG. 3 illustrates a method for solving the problem when PTAA is selected as the photorefractive composite material 5.
- the HOMO of PVCz is ⁇ 5.9 eV and the Fermi level of ITO is ⁇ 4.8 eV as shown on the left side of FIG.
- the potential difference ( ⁇ E FH ) is 1.1 eV.
- the HOMO of PTAA is ⁇ 5.2 eV as shown on the right of FIG. Since the Fermi level is ⁇ 4.8 eV, the energy level difference ( ⁇ E FH ) is as small as 0.4 eV. Therefore, when PTAA is selected, a large dark current is easily generated.
- the dark current control layer 4 is formed on the surface 3a of the ITO electrode 3 to solve the above-mentioned problems.
- the Fermi level of the ITO electrode 3 becomes shallow (upward in the figure) as shown in the left to right diagrams of FIG.
- the Fermi level of the ITO electrode 3 becomes shallow (above)
- the energy level difference between the HOMO of PTAA and the Fermi level increases (from 0.4 eV to 0.9 eV in the figure), Generation of dark current can be suppressed.
- a single monolayer or a plurality of monolayers formed on the surface 3 a of the ITO electrode 3 is suitable for the dark current control layer 4.
- the single-layer monomolecular film or the plurality of monolayers are not necessarily formed uniformly over the entire surface 3 a of the ITO electrode 3. That is, even if the surface 3a of the ITO electrode 3 partially has a region where a single-layer monomolecular film or a plurality of monolayers are not formed, an improvement effect was recognized.
- a part of the surface 3a of the ITO electrode 3 may be a monomolecular film, and the other part of the surface 3a may be a multi-layer monomolecular film.
- a self-assembled monolayer that self-assembles on the ITO electrode 3 is used.
- the single-layer monomolecular film or the plurality of monolayers are not limited to self-assembled monolayers.
- the self-assembled monomolecular film is formed by chemically modifying the inner surface 3a of the transparent electrode 3 with a silane compound.
- a silane compound is not limited, and 3-aminopropyltrimethoxysilane (APTMS) is most preferable.
- Examples of other self-assembled monolayers include trichlorosilanes and dimethylchlorosilanes.
- the self-assembled monomolecular film is a monomolecular film formed by self-assembly or self-assembly, and is a molecular aggregate formed on the solid surface in the process of chemical adsorption of organic molecules. Due to the interaction between adsorbed molecules, the constituent molecules of the aggregate are densely assembled. As a result, a structure having a highly regular molecular orientation and molecular arrangement is spontaneously formed.
- FIG. 4 is a conceptual diagram when a self-assembled monomolecular film (SAM) as the dark current control layer 4 is formed on the ITO electrode substrate 7.
- SAM self-assembled monomolecular film
- a SAM-coated ITO electrode substrate can be obtained.
- the film formation conditions such as the mixing ratio of each component in the hydrophilized solution, the solvent, the immersion time, and the cleaning component when forming the SAM can be appropriately changed according to the type of the transparent electrode. If a self-assembled monomolecular film is formed using the above method, ordered monomolecular films can be obtained, and the effect of suppressing dark current can be improved.
- An integrated precursor molecule that becomes a SAM has a head group and a terminal group. These are connected by a hydrocarbon chain. SAM is formed by dissolving these in a solvent and immersing the surface on which the film is to be formed. Unlike the simple adhesion phenomenon to the surface, the place where the integrated precursor molecules spontaneously form a two-dimensional fine structure on the adsorption surface is called a self-assembled monolayer.
- a self-assembled monolayer In addition to dipping in a liquid as a film forming method, there are a method of evaporating in a high vacuum to form a film, and spraying with a spray or the like.
- the bonding portion can be classified into three types: thiol (mainly HS-group), silane (mainly X3Si-group), and acetic acid (mainly COOH-group). Different substances are adsorbed.
- the properties of the surface after SAM film formation change depending on the end group.
- the methyl group (CH 3 group), amino group (NH 2 group), carboxyl group (COOH group) as the end group, ferrocene, quinone, porphyrin, and the like are variously synthesized depending on the application.
- the thickness of the self-assembled monomolecular film it is preferable that the thickness is one molecule of the silane compound in order to obtain a high dark current suppressing effect.
- the photorefractive polymer element 1 of the present embodiment includes a dissolving step for dissolving the photorefractive polymer in a solvent, a solvent distilling step for distilling off the solvent, and a sandwich type device forming step for forming a sandwich type device. Manufactured by a manufacturing method.
- a photorefractive polymer, a nonlinear optical dye, a plasticizer, and a sensitizer are dissolved in a solvent at a predetermined ratio.
- the solvent is not particularly limited, and tetrahydrofuran (THF), chloroform, N-methylpyrrolidone (NMP), dimethylformamide and the like are used, and THF is preferable.
- THF tetrahydrofuran
- the dissolution temperature may be about room temperature.
- the solution may be stirred as necessary.
- the method of stirring this solution is not limited, and for example, it is performed by a method using a stirrer chip.
- the solvent is removed.
- the method for removing the solvent is not particularly limited, and for example, a cast film may be obtained. Specifically, an ITO electrode is formed on an insulating substrate to obtain an ITO electrode substrate, and then a SAM that is a dark current control layer is formed on the surface of the ITO electrode substrate to obtain a SAM-coated ITO electrode substrate. Then, a solution in which each component is dissolved is cast on the surface, and then the solvent is evaporated at room temperature, followed by natural drying overnight, followed by vacuum drying at about 80 ° C. for 12 hours. Evaporate.
- spacers polyimide, thickness: 50 ⁇ m
- another SAM-coated ITO electrode substrate that has been separately manufactured is placed on top.
- a sandwich-type photorefractive element is produced by pressure bonding with a vacuum press while applying temperature.
- the thickness of the photorefractive composite material in the element is preferably 50 to 100 ⁇ m. If it is less than 50 ⁇ m, it is difficult to satisfy the Bragg diffraction condition, and if it exceeds 100 ⁇ m, the applied voltage may increase or the absorption may increase.
- the photorefractive element obtained by the above manufacturing method is, for example, recording / reproduction of moving images such as video images, real-time holograms, wavefront and phase manipulation of light, pattern recognition, optical amplification, nonlinear optical information processing, super multiplexing It can be used for hologram recording, high-density optical data recording, optical correlation systems, optical computers, and the like.
- the dark current control layers 4 and 4 formed on the inner surfaces 7a and 7a of the pair of ITO electrode substrates 7 and 7 and the photorefractive composite material 5 mainly composed of PTAA are provided.
- the dark current control layer 4 suppresses the generation of dark current and does not cause dielectric breakdown while expressing high responsiveness by PTAA. Thereby, the photorefractive polymer element 1 with significantly improved responsiveness can be obtained.
- the Fermi potential of the ITO electrode 3 is made shallow, and the generation of dark current accompanying the selection of PTAA is efficiently performed. Can be suppressed. Since the self-assembled monomolecular film constituting the dark current control layer 4 is formed by chemically modifying 3-aminopropyltrimethoxysilane on the surface 3a of the ITO electrode 3, generation of dark current is minimized. The limit can be suppressed, and the dielectric breakdown can be surely prevented.
- the photorefractive polymer elements of Examples 1 to 6 were manufactured. SAM was used for the dark current control layers of Examples 1 to 6. The thickness of the photorefractive composite was adjusted to 80 to 115 ⁇ m.
- the components of the photorefractive composite in each example are as follows.
- Photorefractive polymer PTAA / 44% by weight
- Nonlinear optical dye 7-DCST / 35% by weight
- Plasticizer ECz / 20% by weight
- Sensitizer PCBM / 1% by weight
- Photorefractive polymer PTAA / 42% by weight
- Nonlinear optical dye PDCST / 35% by weight
- Plasticizer TAA / 20% by weight
- Sensitizer PCBM / 3 wt%
- Photorefractive polymer PTAA / 44% by weight
- Nonlinear optical dye PDCST / 35% by weight
- Plasticizer TAA / 20% by weight
- Sensitizer PCBM / 1% by weight
- Photorefractive polymer PTAA / 44.5% by weight
- Nonlinear optical dye PDCST / 35% by weight
- Plasticizer TAA / 20% by weight
- Sensitizer PCBM / 0.5% by weight
- Photorefractive polymer PTAA / 44.7% by weight
- Nonlinear optical dye PDCST / 35% by weight
- Plasticizer TAA / 20% by weight
- Sensitizer PCBM / 0.3% by weight
- Photorefractive polymer PTAA / 44.9% by weight
- Nonlinear optical dye PDCST / 35% by weight
- Plasticizer TAA / 20% by weight
- Sensitizer PCBM / 0.1% by weight
- the photorefractive polymer elements of Comparative Examples 1 to 4 were manufactured. In Comparative Example 2 and Comparative Example 3, no dark current control layer was provided, and in Comparative Example 1 and Comparative Example 4, SAM, which was a dark current control layer, was provided. The thickness of the photorefractive composite was adjusted to 80 to 115 ⁇ m.
- the components of the photorefractive composite in each example are as follows.
- Photorefractive polymer PTAA / 45% by weight
- Nonlinear optical dye PDCST / 35% by weight
- Plasticizer TAA / 20% by weight
- Sensitizer PCBM / 0% by weight
- Photorefractive polymer PVCz (Mw: 370000) / 44% by weight
- Nonlinear optical dye 7-DCST / 35% by weight
- Plasticizer ECz / 20% by weight
- Sensitizer TNF / 1% by weight
- Photorefractive polymer PVCz (Mw: 370000) / 44% by weight
- Nonlinear optical dye 7-DCST / 35% by weight
- Plasticizer ECz / 20% by weight
- Sensitizer TNF / 1% by weight
- FIG. 5 is a schematic diagram for explaining a four-wave mixing method (DFWM) for measuring diffraction efficiency (%).
- the diffraction efficiency (%) was measured by a four-wave mixing method with an electric field applied (45 V / ⁇ m) to the photorefractive polymer element.
- a 632.8 nm He—Ne laser was used for the measurement.
- the diffraction efficiency (%) generated by the photorefractive effect, that is, the refractive index change magnitude ⁇ n can be evaluated from the Bragg diffraction intensity measurement (diffraction efficiency measurement).
- the diffraction efficiency can be measured by making low-power probe light incident on the sample film in which the refractive index grating is generated by the writing light and measuring the intensity of light diffracted by the refractive index grating.
- the normalized diffraction efficiency ⁇ norm is shown and evaluated by the following equation (1).
- the diffraction efficiency is measured by inclining the photorefractive polymer element so that the angle ⁇ between the normal H of the photorefractive polymer element (Sample) and the bisector of the two interference beams is 50 °.
- the normalized diffraction efficiency ⁇ norm can be related to the magnitude of refractive index change: ⁇ n by Kugelnick's coupled wave theory in a thick medium.
- the normalized diffraction efficiency ⁇ norm and the refractive index change magnitude ⁇ n can be approximately expressed by one expression, and the refractive index change magnitude ⁇ n can be evaluated from the normalized diffraction efficiency ⁇ norm .
- the intensity I diffracted of the diffracted light is a high-speed bench meter (for example, manufactured by Agilent; 34411 digital multimeter), and the transmitted light intensity I transmitted is the high-speed bench meter (for example, manufactured by Agilent; 34411 digital Measure using a multimeter.
- Table 1 shows the measurement results of diffraction efficiency and response time.
- FIG. 6 shows a graph showing the relationship between the electric field intensity and diffraction efficiency of Example 1
- FIG. 7 shows a graph showing the time response of the diffraction efficiency of Example 1
- FIG. 8 shows the relationship between the applied electric field and dark current.
- the graph to represent is shown. From FIG. 6, the diffraction efficiency was 6% at 25 V / ⁇ m.
- FIG. 7 shows a time-resolved diffraction efficiency of 20 V / ⁇ m. The response speed at this time was 11.3 ms ( ⁇ value in the figure indicates dispersion).
- ⁇ value in the figure indicates dispersion
- FIG. 9 is a graph showing the relationship between the concentration of PCBM as a sensitizer, the external diffraction efficiency, and the grating formation speed.
- FIG. 10 is a graph showing the relationship between the concentration of PCBM as a sensitizer and sensitivity.
- Sensitivity S represented by the following formula (5) can be used as an index of photorefractive performance. The sensitivity S increases as the diffraction efficiency increases, the laser energy per unit area decreases, and the response time decreases. That is, the higher sensitivity S means that the hologram image becomes brighter and the speed at which the hologram image is formed increases.
- the photorefractive composite material of the photorefractive polymer element may contain other components in addition to the above components within a range not impairing the photorefractive property.
- examples of such other components include an antioxidant and an ultraviolet absorber.
- the invention includes an insulating substrate, a transparent electrode formed on one surface of the insulating substrate, a dark current control layer formed on the surface of the transparent electrode, and a transparent electrode and a dark current control layer formed on the insulating substrate.
- a photorefractive composite material provided through a high-speed responsive photorefractive polymer element.
- the present invention can be of any form as long as it is a fast response photorefractive polymer element in which a dark current control layer is interposed between the transparent electrode on the transparent electrode substrate and the photorefractive composite material. There may be.
- ITO electrodes have been used for photorefractive polymer elements because side chain carbazole and side chain triphenylamine-based HOMOs are sufficiently deeper than ITO.
- the photorefractive polymer element is required to have further high-speed response, and the demand for the photorefractive polymer element provided with the SAM as in the present invention is expected to increase.
- indium which is the main component of ITO, is a rare metal, and its stable supply is feared, and its price is expected to rise. Therefore, when considering industrialization, selection of a transparent electrode other than the ITO electrode is desired from the viewpoint of cost and environment.
- ITO As an alternative material for ITO, some of them are listed above, but ZnO: ⁇ 5.8 eV (Fermi level), Ga 2 O 3 / ZnO: ⁇ 5.1 eV, GaN: ⁇ 5.5 eV, MgO / C: Unknown, graphene sheet: -4.4 eV, PEDOT / PPS: -5.8 eV, and the like. These have deeper Fermi levels than ITO: -4.8 eV, and are not suitable for photorefractive polymer elements in the prior art. However, by applying the present invention, it is possible to select such an ITO substitute material, and the present invention is considered to greatly contribute to the information industry and the like.
- Photorefractive polymer element 1 Photorefractive polymer element 2 Insulating substrate 3 Transparent electrode (ITO electrode) 4 Dark current control layer (SAM) 5 Photorefractive composite material 6 Spacer 7 Transparent electrode substrate
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Abstract
Description
増感剤は、電子受容体としての性能を有しており、フォトリフラクティブ性を高めるために配合されるものである。増感剤が配合されると、当該増感剤とフォトリフラクティブポリマーとにより、電荷移動錯体が形成され、有用なフォトリフラクティブ性が発現される。
非線形光学色素とは、2次の非線形光学特性を示すドナーアクセプター型分子、即ち、電場によって屈折率が変化する材料(2次非線形光学材料)のことである。本実施形態では、非線形光学色素として下記式(3)で表される[[4-(ヘキサヒドロ-1H-アゼピン-1-イル)フェニル]メチレン]プロパンジニトリル(7-DCST)を用いている。
可塑剤は、マトリックスのガラス転移温度を低下させる役割を果たす。本実施形態では、増感剤として下記式(6)で表されるエチルカルバゾール(ECz)を用いている。
フォトリフラクティブポリマーは限定されないが、本実施形態で用いる下記式(1)で表されるトリアリールアミン系非結晶質高分子のポリトリアリールアミン(PTAA):Poly[bis(4-phenyl)(2,4,6-trimethylphenyl)amine]が好ましい。これは、ポリトリアリールアミン半導体(Polytriarylamine Semiconductors)ともよばれる。
本実施形態の各暗電流制御層4は、各透明電極基板7(ITO電極基板)の内表面7aに形成されており、当該内表面7aを覆っている。従って、各透明電極基板7とフォトリフラクティブ複合材料5との間に各暗電流制御層4が介在しており、各透明電極3とフォトリフラクティブ複合材料5とは接触していない状態となっている。暗電流制御層4は、各透明電極基板7の双方に形成することが好ましいが、発現する性能に応じて何れかの透明電極基板のみに形成してもよい。
フォトリフラクティブポリマー:PTAA/44重量%
非線形光学色素:7-DCST/35重量%
可塑剤:ECz/20重量%
増感剤:PCBM/1重量%
フォトリフラクティブポリマー:PTAA/42重量%
非線形光学色素:PDCST/35重量%
可塑剤:TAA/20重量%
増感剤:PCBM/3重量%
フォトリフラクティブポリマー:PTAA/44重量%
非線形光学色素:PDCST/35重量%
可塑剤:TAA/20重量%
増感剤:PCBM/1重量%
フォトリフラクティブポリマー:PTAA/44.5重量%
非線形光学色素:PDCST/35重量%
可塑剤:TAA/20重量%
増感剤:PCBM/0.5重量%
フォトリフラクティブポリマー:PTAA/44.7重量%
非線形光学色素:PDCST/35重量%
可塑剤:TAA/20重量%
増感剤:PCBM/0.3重量%
フォトリフラクティブポリマー:PTAA/44.9重量%
非線形光学色素:PDCST/35重量%
可塑剤:TAA/20重量%
増感剤:PCBM/0.1重量%
フォトリフラクティブポリマー:PTAA/45重量%
非線形光学色素:PDCST/35重量%
可塑剤:TAA/20重量%
増感剤:PCBM/0重量%
フォトリフラクティブポリマー:PTAA/45重量%
非線形光学色素:7-DCST/35重量%
可塑剤:ECz/20重量%
増感剤:PCBM/0重量%
フォトリフラクティブポリマー:PVCz(Mw:370000)/44重量%
非線形光学色素:7-DCST/35重量%
可塑剤:ECz/20重量%
増感剤:TNF/1重量%
フォトリフラクティブポリマー:PVCz(Mw:370000)/44重量%
非線形光学色素:7-DCST/35重量%
可塑剤:ECz/20重量%
増感剤:TNF/1重量%
図5は回折効率(%)を測定するための4光波混合法(DFWM)を説明するための概略図である。回折効率(%)の測定は、フォトリフラクティブポリマー素子に電界を印加(45V/μm)した状態で4光波混合法によって測定した。測定には632.8nmのHe-Neレーザーを用いた。フォトリフラクティブ効果によって生じる回折効率(%)、即ち屈折率変化の大きさΔnは、ブラッグ回折の強度測定(回折効率測定)から評価することができる。書き込み光により屈折率格子を生じた試料フィルムに、ブラッグ条件で低出力のプローブ光を入射させて、屈折率格子により回折する光の強度を測定することによって、その回折効率を測定することができる。ここでは規格化回折効率ηnormについて示し、次式(1)により評価する。フォトリフラクティブポリマー素子(Sample)の法線Hと2本の干渉ビームの2等分線との間の角度θが50°となるように、フォトリフラクティブポリマー素子を傾けて回折効率を測定する。
応答時間は、次式(2)に示すKohlrausch-Williams-Watts(KWW)式によるフィッティングで算出された値を用いた。η:回折効率、η0:飽和回折効率、t:時間、τ:応答時間、β(0<β≦1):分散を示す。
2 絶縁基板
3 透明電極(ITO電極)
4 暗電流制御層(SAM)
5 フォトリフラクティブ複合材料
6 スペーサー
7 透明電極基板
Claims (10)
- 絶縁基板と、
この絶縁基板の片面上に形成された透明電極と、
この透明電極の表面に形成された暗電流制御層と、
前記絶縁基板上で前記透明電極及び暗電流制御層を介して設けられたフォトリフラクティブ複合材料と、
を備えることを特徴とする高速応答性フォトリフラクティブポリマー素子。 - 前記絶縁基板に略平行状に配置された他の絶縁基板と、
前記他の絶縁基板の内面上に形成された他の透明電極と、
前記他の透明電極の内表面上に形成された他の暗電流制御層と、
をさらに備え、
前記フォトリフラクティブ複合材料が前記一対の絶縁基板間で前記各透明電極及び各暗電流制御層を介して挟持されていることを特徴とする請求項1に記載の高速応答性フォトリフラクティブポリマー素子。 - 前記暗電流制御層は、前記透明電極の表面に形成された単一層の単分子膜又複数層の単分子膜であることを特徴とする請求項1に記載の高速応答性フォトリフラクティブポリマー素子。
- 前記単一層の単分子膜又複数層の単分子膜は、前記透明電極の表面にシラン化合物を化学修飾して形成されたものであることを特徴とする請求項3に記載の高速応答性フォトリフラクティブポリマー素子。
- 前記シラン化合物は、3-アミノプロピルトリメトキシシランであることを特徴とする請求項4に記載の高速応答性フォトリフラクティブポリマー素子。
- 前記単一層の単分子膜又複数層の単分子膜は、前記透明電極が前記絶縁基板上に形成された透明電極基板を、アンモニア水及び過酸化水素の混合溶液中、又はピラニア溶液中に浸漬させて親水化し、この親水化電極基板を、3-アミノプロピルトリメトキシシラン混合溶媒中に浸漬させて集積化前駆体を生成し、この集積化前駆体の表面をアルコールで洗浄して余剰分子を除去することによって形成されたものであることを特徴とする請求項5に記載の高速応答性フォトリフラクティブポリマー素子。
- 前記単一層の単分子膜又複数層の単分子膜の膜厚はシラン化合物の1分子分以上の厚みであることを特徴とする請求項6に記載の高速応答性フォトリフラクティブポリマー素子。
- 前記フォトリフラクティブ複合材料は、非線形光学色素と、増感剤と、可塑剤と、を含んでいることを特徴とする請求項8に記載の高速応答性フォトリフラクティブポリマー素子。
- 前記フォトリフラクティブポリマーが10~50重量%、前記非線形光学色素が20~50重量%、前記増感剤が0.1~3重量%、前記可塑剤が10~40重量%含まれていることを特徴とする請求項9に記載の高速応答性フォトリフラクティブポリマー素子。
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TAKASHI FUJIWARA ET AL.: "Andenryu Seigyo ni yoru Photorefractive Polymer no Kosokuka", DAI 73 KAI EXTENDED ABSTRACTS; THE JAPAN SOCIETY OF APPLIED PHYSICS, 27 August 2012 (2012-08-27), pages 12 - 102 * |
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