WO2021152976A1 - コレステリック液晶膜 - Google Patents
コレステリック液晶膜 Download PDFInfo
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- WO2021152976A1 WO2021152976A1 PCT/JP2020/043477 JP2020043477W WO2021152976A1 WO 2021152976 A1 WO2021152976 A1 WO 2021152976A1 JP 2020043477 W JP2020043477 W JP 2020043477W WO 2021152976 A1 WO2021152976 A1 WO 2021152976A1
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3016—Polarising elements involving passive liquid crystal elements
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- C—CHEMISTRY; METALLURGY
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- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/36—Steroidal liquid crystal compounds
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- C09K19/00—Liquid crystal materials
- C09K19/52—Liquid crystal materials characterised by components which are not liquid crystals, e.g. additives with special physical aspect: solvents, solid particles
- C09K19/58—Dopants or charge transfer agents
- C09K19/586—Optically active dopants; chiral dopants
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
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- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/06—Non-steroidal liquid crystal compounds
- C09K19/34—Non-steroidal liquid crystal compounds containing at least one heterocyclic ring
- C09K19/3491—Non-steroidal liquid crystal compounds containing at least one heterocyclic ring having sulfur as hetero atom
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- C09K19/00—Liquid crystal materials
- C09K19/52—Liquid crystal materials characterised by components which are not liquid crystals, e.g. additives with special physical aspect: solvents, solid particles
- C09K19/54—Additives having no specific mesophase characterised by their chemical composition
- C09K19/56—Aligning agents
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/10—Esters of organic acids
- C08J2301/12—Cellulose acetate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K2019/0444—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit characterized by a linking chain between rings or ring systems, a bridging chain between extensive mesogenic moieties or an end chain group
- C09K2019/0448—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit characterized by a linking chain between rings or ring systems, a bridging chain between extensive mesogenic moieties or an end chain group the end chain group being a polymerizable end group, e.g. -Sp-P or acrylate
Definitions
- This disclosure relates to a cholesteric liquid crystal film.
- the cholesteric liquid crystal layer is known as a layer having a property of selectively reflecting either right-handed circularly polarized light or left-handed circularly polarized light in a specific wavelength range, for example.
- the cholesteric liquid crystal layer developed for various uses is used as, for example, a projected image display member (for example, a reflecting element). Recently, attempts have been made to impart reflection anisotropy to the cholesteric liquid crystal layer (see, for example, Patent Document 1).
- a plurality of cholesteric liquid crystal layers may be combined.
- the wavelength of light reflected by the cholesteric liquid crystal layer depends on the spiral pitch (the length of the spiral axis per rotation of the spiral; the same applies hereinafter). Therefore, for example, a plurality of cholesteric liquid crystal layers having different spiral pitches. By using, the wavelength range of the reflectable light can be widened.
- One aspect of the present disclosure is to provide a cholesteric liquid crystal film with a small haze.
- the distance between two adjacent dark portions among the dark portions observed in the second cholesteric liquid crystal layer is the distance between the dark portions observed in the first cholesteric liquid crystal layer.
- the cholesteric liquid crystal film according to ⁇ 1> which is different from the distance between two adjacent dark areas.
- the distance between two adjacent dark parts among the dark parts observed in the second cholesteric liquid crystal layer is the distance between the two adjacent dark parts observed in the first cholesteric liquid crystal layer.
- the cholesteric liquid crystal film according to ⁇ 1> or ⁇ 2> which is larger than the distance between two adjacent dark areas.
- the dark portion observed in the second cholesteric liquid crystal layer is adjacent to the distance between two adjacent dark portions in the dark portion observed in the first cholesteric liquid crystal layer.
- the distance between two adjacent dark portions among the dark portions observed in the first cholesteric liquid crystal layer is 0.1 ⁇ m to 2 ⁇ m.
- the distance between two adjacent dark portions among the dark portions observed in the second cholesteric liquid crystal layer is 0.1 ⁇ m to 5 ⁇ m.
- the cholesteric according to any one of ⁇ 1> to ⁇ 6>, wherein the ratio of the dark part to be formed is 50% to 100% with respect to the number of the dark parts observed in the second cholesteric liquid crystal layer. Liquid crystal film.
- the dark portion observed in the first cholesteric liquid crystal layer is inclined with respect to the main surface of the first cholesteric liquid crystal layer, and the second cholesteric liquid crystal layer is inclined.
- the cholesteric liquid crystal film according to any one of ⁇ 1> to ⁇ 7>, wherein the dark portion observed in the cholesteric liquid crystal layer is inclined with respect to the main surface of the second cholesteric liquid crystal layer.
- the average angle of the dark portion observed in the first cholesteric liquid crystal layer is 20 ° to 90 ° with respect to the main surface of the first cholesteric liquid crystal layer.
- the striped pattern of the first cholesteric liquid crystal layer is observed at least in a cross section in the thickness direction of the first cholesteric liquid crystal layer, and the striped pattern of the second cholesteric liquid crystal layer is observed.
- a cholesteric liquid crystal film having a small haze is provided.
- the numerical range indicated by using "-" indicates a range including the numerical values before and after "-" as the lower limit value and the upper limit value, respectively.
- the upper limit value or the lower limit value described in a certain numerical range may be replaced with the upper limit value or the lower limit value of another numerical range described stepwise.
- the upper limit value or the lower limit value described in a certain numerical range may be replaced with the value shown in the examples.
- the amount of each component in the composition means the total amount of the plurality of substances present in the composition when a plurality of substances corresponding to each component are present in the composition, unless otherwise specified. ..
- process is included in the term “process” as long as the intended purpose of the process is achieved, not only in an independent process but also in cases where it cannot be clearly distinguished from other processes. ..
- ordinal numbers are terms used to distinguish a plurality of components, and limit the number of components and the superiority or inferiority of the components. is not it.
- the "cross section in the thickness direction” means a surface that appears by cutting an object along the thickness direction.
- main surface of the liquid crystal layer used with respect to the cross-sectional view in the thickness direction refers to two surfaces (that is, the upper surface) of the liquid crystal layer intersecting the thickness direction in the cross-sectional view in the thickness direction. And the lower surface) are used as a term to refer to at least one surface.
- the "molecular axis” means an axis that passes through the center of the molecular structure along the longitudinal direction of the molecular structure.
- the "molecular axis” used for the disk-shaped liquid crystal compound means an axis that intersects the disk surface of the disk-shaped liquid crystal compound at right angles.
- solid content means a component obtained by removing a solvent from all the components of an object.
- the "solid content mass” means the mass obtained by subtracting the mass of the solvent from the mass of the object.
- the cholesteric liquid crystal film according to the present disclosure is arranged in contact with the first cholesteric liquid crystal layer having a striped pattern in which dark parts and bright parts are alternately arranged, which is observed using a microscope, and the first cholesteric liquid crystal layer. It has a second cholesteric liquid crystal layer having a striped pattern in which dark parts and bright parts are alternately arranged, which is observed using a microscope, and is an interface between the first cholesteric liquid crystal layer and the second cholesteric liquid crystal layer. In, the dark portion observed in the second cholesteric liquid crystal layer is connected to the dark portion observed in the first cholesteric liquid crystal layer. According to one aspect of the present disclosure described above, a cholesteric liquid crystal film having a small haze is provided.
- the cholesteric liquid crystal film according to the present disclosure exerts the above effect is presumed as follows.
- the orientation of the liquid crystal for example, the orientation of the liquid crystal compound
- the change in the refractive index becomes large locally, so that the light is scattered and the haze becomes large.
- the dark portion observed in the second cholesteric liquid crystal layer is the first cholesteric.
- the first cholesteric liquid crystal layer may be referred to as a "first liquid crystal layer”
- the second cholesteric liquid crystal layer may be referred to as a "second liquid crystal layer”.
- the first cholesteric liquid crystal layer and the second cholesteric liquid crystal layer are collectively referred to as a "liquid crystal layer”. In some cases.
- the cholesteric liquid crystal film according to the present disclosure has a first cholesteric liquid crystal layer having a striped pattern in which dark parts and bright parts are alternately arranged, which is observed using a microscope.
- Cholesteric liquid crystal which is known as a form of liquid crystal, has a spiral structure formed by spirally arranging a plurality of liquid crystal compounds.
- the orientation of the molecular axis of the liquid crystal compound in the helical structure changes along the helical axis. Therefore, when the cholesteric liquid crystal is observed using a microscope, the dark part (referred to as a region that looks relatively dark; the same applies hereinafter) and the bright part (relatively) depending on the direction of the molecular axis of the liquid crystal compound with respect to the observation direction. An area that looks bright. The same shall apply hereinafter.) Is observed.
- a scanning electron microscope or a polarizing microscope is used as the microscope for observing the dark part and the bright part.
- the striped pattern of the first liquid crystal layer may be observed on the surface of the first liquid crystal layer (for example, the surface of the first liquid crystal layer opposite to the surface in contact with the second liquid crystal layer).
- the striped pattern of the first liquid crystal layer may be observed in the cross section of the first liquid crystal layer.
- the striped pattern of the first liquid crystal layer is preferably observed at least in the cross section of the first liquid crystal layer in the thickness direction.
- the sample used for cross-section observation may be prepared by using, for example, a microtome.
- the dark portion observed in the first liquid crystal layer is preferably inclined with respect to the main surface of the first liquid crystal layer.
- the aspect that "the dark part is inclined with respect to the main surface of the liquid crystal layer” is not limited to the state where the dark part is inclined with respect to the main surface of the liquid crystal layer, and the dark part is the main surface of the liquid crystal layer. It includes a state of being orthogonal to the surface (that is, the angle between the dark part and the main surface of the liquid crystal layer is 90 °).
- the dark portion observed in the first liquid crystal layer is inclined, so that the bright portion and the dark portion are substantially orthogonal to the arrangement direction.
- the spiral axis also tilts. Therefore, when the angle between the direction of light incident on the first liquid crystal layer from an oblique direction (that is, the incident direction) and the spiral axis is small, the reflecting surface derived from the cholesteric liquid crystal (that is, orthogonal to the spiral axis) is formed.
- a plane in which the directions of the molecular axes of the liquid crystal compounds existing on the same plane are the same; the same applies hereinafter) increases the degree of circular polarization of the light.
- the dark portion observed in the first liquid crystal layer is inclined with respect to the main surface of the first liquid crystal layer (hereinafter, referred to as "inclination of the dark portion" in this paragraph). May be observed in at least one cross-sectional view in the thickness direction of the liquid crystal layer. For example, even if the inclination of the dark portion is not observed in any one cross-sectional view, the inclination of the dark portion may be observed in the other cross-sectional view.
- the angle of the dark part observed in the first liquid crystal layer is not limited.
- the average angle of the dark portion observed in the first liquid crystal layer is 5 ° with respect to the main surface of the first liquid crystal layer from the viewpoint of the uniformity of the inclination angle of the spiral axis. It is preferably more than that, more preferably 10 ° or more, and particularly preferably 20 ° or more.
- the average angle of the dark portion observed in the first liquid crystal layer is preferably 90 ° or less with respect to the main surface of the first liquid crystal layer.
- the average angle of the dark part observed in the first liquid crystal layer in the cross-sectional view in the thickness direction is measured by the following method.
- the angle formed by the main surface of the first liquid crystal layer (hereinafter referred to as "tilt angle") is measured. Unless the tilt angle is 90 °, an angle smaller than a right angle (that is, an acute angle) is adopted as the tilt angle.
- the inclination angle is measured for a total of five dark areas. The value obtained by arithmetically averaging the measured values is taken as the average angle of the dark part observed in the first liquid crystal layer.
- the distance between the dark part observed in the first liquid crystal layer is not limited.
- the distance between two adjacent dark portions among the dark portions observed in the first liquid crystal layer is preferably 0.01 ⁇ m or more, more preferably 0.05 ⁇ m or more. It is particularly preferably 0.1 ⁇ m or more.
- the distance between two adjacent dark parts among the dark parts observed in the first liquid crystal layer is preferably 500 ⁇ m or less, more preferably 100 ⁇ m or less, and 10 ⁇ m or less. It is more preferably 2 ⁇ m or less, and particularly preferably 2 ⁇ m or less.
- the distance between two adjacent dark areas may be referred to as "distance between dark areas”.
- the distance between two adjacent dark parts among the dark parts observed in the first liquid crystal layer is measured by the following method. Based on the cross-sectional image of the first liquid crystal layer in the thickness direction obtained by using a scanning electron microscope or a polarizing microscope, five sets of two adjacent dark parts composed of a total of six dark parts are selected, and 5 The shortest distance between two adjacent dark areas in each of the sets is measured. More specifically, as the shortest distance between two adjacent dark parts in the first set, the shortest distance between the center in the width direction of one dark part and the center in the width direction of one dark part adjacent to the dark part. To measure.
- the shortest distance between the two adjacent dark areas from the second group to the fifth group is measured according to the above method.
- the arithmetic mean of the measured values is the distance between two adjacent dark areas of the dark areas observed in the first liquid crystal layer.
- the liquid crystal compounds observed on the surface of the first liquid crystal layer opposite to the surface in contact with the second liquid crystal layer are arranged while being twisted along one of the in-plane directions of the first liquid crystal layer. It is preferable to have.
- the linearity of the dark part and the bright part observed in the cross section in the thickness direction becomes high, so that the haze of the cholesteric liquid crystal film can be further reduced.
- the liquid crystal compounds are arranged while twisting along one of the in-plane directions of the liquid crystal layer.
- a striped pattern in which bright parts and dark parts are alternately arranged is observed along one of the in-plane directions of the liquid crystal layer.
- the direction of the molecular axis of the liquid crystal compound changes as the liquid crystal compound proceeds in the above one direction. Therefore, a striped pattern in which bright areas and dark areas are alternately arranged is observed.
- the thickness of the first liquid crystal layer is not limited.
- the average thickness of the first liquid crystal layer is 0. From the viewpoint of suppressing the influence of the smoothness of the surface shape of the layer adjacent to the first liquid crystal layer (for example, the base material and the second liquid crystal layer). It is preferably 1 ⁇ m or more, more preferably 0.5 ⁇ m or more, and particularly preferably 1 ⁇ m or more. From the viewpoint of transparency, the average thickness of the first liquid crystal layer is preferably 500 ⁇ m or less, more preferably 100 ⁇ m or less, and particularly preferably 20 ⁇ m or less.
- the average thickness of the first liquid crystal layer is measured by the following method.
- the thickness at five points is measured based on a cross-sectional image of the first liquid crystal layer in the thickness direction obtained by using a scanning electron microscope or a polarizing microscope.
- the value obtained by arithmetically averaging the measured values is taken as the average thickness of the first liquid crystal layer.
- composition The composition of the first liquid crystal layer is not limited as long as a striped pattern in which dark areas and bright areas are alternately arranged is observed.
- the components of the first liquid crystal layer will be specifically described.
- the first liquid crystal layer preferably contains a liquid crystal compound.
- the type of liquid crystal compound is not limited.
- As the liquid crystal compound for example, a known liquid crystal compound that forms a cholesteric liquid crystal can be used.
- the liquid crystal compound may have a polymerizable group.
- the liquid crystal compound may have one kind alone or two or more kinds of polymerizable groups.
- the liquid crystal compound may have two or more polymerizable groups of the same type.
- the liquid crystal compound can be polymerized. By polymerizing the liquid crystal compound, the stability of the cholesteric liquid crystal can be improved.
- Examples of the polymerizable group include a group having an ethylenically unsaturated double bond, a cyclic ether group, and a nitrogen-containing heterocyclic group capable of causing a ring-opening reaction.
- Examples of the group having an ethylenically unsaturated double bond include an acryloyl group, a methacryloyl group, an acryloyloxy group, a methacryloyloxy group, a vinyl group, a vinylphenyl group, and an allyl group.
- Examples of the cyclic ether group include an epoxy group and an oxetanyl group.
- Examples of the nitrogen-containing heterocyclic group capable of causing a ring-opening reaction include an aziridinyl group.
- the polymerizable group is preferably at least one selected from the group consisting of a group having an ethylenically unsaturated double bond and a cyclic ether group.
- the polymerizable group is at least selected from the group consisting of an acryloyl group, a methacryloyl group, an acryloyloxy group, a methacryloyloxy group, a vinyl group, a vinylphenyl group, an allyl group, an epoxy group, an oxetanyl group, and an aziridinyl group.
- It is preferably one kind, and more preferably at least one kind selected from the group consisting of an acryloyl group, a methacryloyl group, an acryloyloxy group, and a methacryloyloxy group, and more preferably a group consisting of an acryloyloxy group and a methacryloyloxy group. It is particularly preferable that it is at least one selected more.
- Liquid crystal compounds are classified into, for example, rod-shaped liquid crystal compounds and disk-shaped liquid crystal compounds according to their chemical structure.
- the rod-shaped liquid crystal compound is known as a liquid crystal compound having a rod-shaped chemical structure.
- a known rod-shaped liquid crystal compound can be used.
- the disk-shaped liquid crystal compound is known as a liquid crystal compound having a disk-shaped chemical structure.
- a known disk-shaped liquid crystal compound can be used.
- the liquid crystal compound is preferably a rod-shaped liquid crystal compound, and more preferably a rod-shaped thermotropic liquid crystal compound.
- the rod-shaped thermotropic liquid crystal compound is a compound having a rod-shaped chemical structure and exhibiting liquid crystallinity in a specific temperature range.
- a known rod-shaped thermotropic liquid crystal compound can be used as the rod-shaped thermotropic liquid crystal compound.
- rod-shaped thermotropic liquid crystal compound examples include "Makromol. Chem., 190, 2255 (1989)", “Advanced Materials, 5, 107 (1993)", US Pat. No. 4,683,327, USA.
- Japanese Patent No. 5622648, US Pat. No. 5,770,107 International Publication No. 95/22586, International Publication No. 95/24455, International Publication No. 97/00600, International Publication No. 98/23580, International Publication No. 98 / 52905, Japanese Patent Application Laid-Open No. 1-272551, Japanese Patent Application Laid-Open No. 6-16616, Japanese Patent Application Laid-Open No. 7-110469, Japanese Patent Application Laid-Open No.
- thermotropic liquid crystal compound examples include the liquid crystal compound represented by the general formula 1 in JP-A-2016-81035 and the general formula (I) or the general formula (II) in JP-A-2007-279688. The compounds to be used are also mentioned.
- the rod-shaped thermotropic liquid crystal compound is preferably a compound represented by the following general formula (1).
- Q 1 and Q 2 each independently represent a polymerizable group
- L 1 , L 2 , L 3 and L 4 independently represent a single bond or 2 respectively.
- Representing a valent linking group A 1 and A 2 each independently represent a divalent hydrocarbon group having 2 to 20 carbon atoms, and M represents a mesogen group.
- Examples of the polymerizable group represented by Q 1 and Q 2 in the general formula (1) include the above-mentioned polymerizable group.
- the preferred embodiments of the polymerizable group represented by Q 1 and Q 2 are the same as the preferred embodiments of the polymerizable group described above.
- the divalent linking groups represented by L 1 , L 2 , L 3 , and L 4 are -O-, -S-, -CO-, -NR-, and -CO-O.
- -, -O-CO-O-, -CO-NR-, -NR-CO-, -O-CO-, -O-CO-NR-, -NR-CO-O-, and NR-CO-NR It is preferably a divalent linking group selected from the group consisting of ⁇ .
- R in the above-mentioned divalent linking group represents an alkyl group having 1 to 7 carbon atoms or a hydrogen atom.
- At least one of L 3 and L 4 is preferably —O—CO—O ⁇ .
- the divalent hydrocarbon group having 2 to 20 carbon atoms represented by A 1 and A 2 has an alkylene group having 2 to 12 carbon atoms and a carbon atom number. It is preferably an alkenylene group having 2 to 12 or an alkynylene group having 2 to 12 carbon atoms, and more preferably an alkylene group having 2 to 12 carbon atoms.
- the divalent hydrocarbon group is preferably in the form of a chain.
- the divalent hydrocarbon group may contain oxygen atoms that are not adjacent to each other or sulfur atoms that are not adjacent to each other.
- the divalent hydrocarbon group may have a substituent. Substituents include, for example, halogen atoms (eg, fluorine, chlorine, and bromine), cyano groups, methyl groups, and ethyl groups.
- the mesogen group represented by M is a group that forms the main skeleton of a liquid crystal compound that contributes to liquid crystal formation.
- the mesogen group represented by M for example, the description (particularly, pages 7 to 16) of "Flusige Editorial in Table II" (VEB, Editorial, fur, Grundstoff, Industrie, Leipzig, 1984), and liquid crystal (pages 7 to 16). You can refer to the description (especially Chapter 3) of the Handbook Editorial Committee, edited by Maruzen, 2000).
- the mesogen group represented by M is a group containing at least one cyclic structure selected from the group consisting of an aromatic hydrocarbon group, a heterocyclic group, and an alicyclic hydrocarbon group. It is preferably a group containing an aromatic hydrocarbon group, and more preferably a group containing an aromatic hydrocarbon group.
- the mesogen group represented by M is preferably a group containing 2 to 5 aromatic hydrocarbon groups, and is a group containing 3 to 5 aromatic hydrocarbon groups. Is more preferable.
- the mesogen group represented by M is preferably a group containing 3 to 5 phenylene groups and the phenylene groups are linked to each other by -CO-O-.
- the cyclic structure (for example, aromatic hydrocarbon group, heterocyclic group, and alicyclic hydrocarbon group) contained in the mesogen group represented by M may have a substituent. good.
- the substituent include an alkyl group having 1 to 10 carbon atoms (for example, a methyl group).
- rod-shaped thermotropic liquid crystal compounds are shown below.
- the rod-shaped thermotropic liquid crystal compound is not limited to the compounds shown below.
- the liquid crystal compound may be a synthetic product synthesized by a known method or a commercially available product.
- Commercially available liquid crystal compounds are available from, for example, Tokyo Chemical Industry Co., Ltd. and Merck & Co., Inc.
- the first liquid crystal layer may contain one kind alone or two or more kinds of liquid crystal compounds.
- the content of the liquid crystal compound in the first liquid crystal layer is preferably 70% by mass or more, and preferably 80% by mass or more, based on the total mass of the first liquid crystal layer. It is more preferably 90% by mass or more, and particularly preferably 90% by mass or more.
- the upper limit of the content of the liquid crystal compound is not limited.
- the content of the liquid crystal compound in the first liquid crystal layer may be determined in the range of 100% by mass or less with respect to the total mass of the first liquid crystal layer.
- the content of the liquid crystal compound in the first liquid crystal layer is less than 100% by mass and 99% by mass with respect to the total mass of the first liquid crystal layer. It may be less than or equal to 96% by mass or less.
- the first liquid crystal layer may contain components other than the liquid crystal compound (hereinafter, referred to as "other components" in this paragraph).
- Other components include, for example, chiral agents, solvents, orientation regulators, polymerization initiators, leveling agents, orientation aids, and sensitizers.
- the cholesteric liquid crystal film according to the present disclosure has a second cholesteric liquid crystal layer which is arranged in contact with the first cholesteric liquid crystal layer and has a striped pattern in which dark parts and bright parts observed by a microscope are alternately arranged.
- the striped pattern of the second liquid crystal layer may be observed on the surface of the second liquid crystal layer (for example, the surface of the second liquid crystal layer opposite to the surface in contact with the first liquid crystal layer).
- the striped pattern of the second liquid crystal layer may be observed in the cross section of the second liquid crystal layer.
- the striped pattern of the second liquid crystal layer is preferably observed at least in the cross section of the second liquid crystal layer in the thickness direction.
- the dark portion observed in the second liquid crystal layer is connected to the dark portion observed in the first liquid crystal layer (hereinafter, "dark portion”).
- connection means a liquid crystal layer obtained by using a scanning electron microscope or a polarizing microscope. In the cross-sectional image in the thickness direction of the above, it means that the dark part observed in the second liquid crystal layer appears to be connected to the dark part observed in the first liquid crystal layer, and it is necessary that both are strictly connected. It's not a thing.
- FIG. 1 is a schematic cross-sectional view showing an example of a cholesteric liquid crystal film according to the present disclosure.
- the cholesteric liquid crystal film 10 shown in FIG. 1 has a first cholesteric liquid crystal layer 20 and a second cholesteric liquid crystal layer 21.
- the first cholesteric liquid crystal layer 20 and the second cholesteric liquid crystal layer 21 are arranged along the stacking direction Z.
- the stacking direction Z is parallel to the thickness direction of the cholesteric liquid crystal film 10.
- the dark portion 30 is inclined with respect to the main surface of the first cholesteric liquid crystal layer 20.
- the dark portion 30 extends in one of the directions orthogonal to the stacking direction Z toward one of the stacking directions Z.
- the second cholesteric liquid crystal layer 21 is arranged in contact with the first cholesteric liquid crystal layer 20.
- a striped pattern in which dark portions 31 and bright portions 41 are alternately arranged is observed.
- the dark portion 31 is inclined with respect to the main surface of the second cholesteric liquid crystal layer 21.
- the dark portion 31 extends in one of the directions orthogonal to the stacking direction Z toward one of the stacking directions Z.
- the dark portion 31 observed in the second cholesteric liquid crystal layer 21 is connected to the dark portion 30 observed in the first cholesteric liquid crystal layer 20. is doing.
- connection rate of dark areas may be referred to as "connection rate of dark areas"
- connection rate of dark areas preferably 50% to 100%, and preferably 70% to 100%, based on the number of dark areas observed in the second liquid crystal layer. More preferably, it is particularly preferably 80% to 100%.
- connection rate of the dark part is measured by the following method. Using a scanning electron microscope or a polarizing microscope, three cross-sectional images in the thickness direction of the liquid crystal layer are acquired. At the interface between the first liquid crystal layer and the second liquid crystal layer observed in each cross-sectional image, the dark portion observed in the second liquid crystal layer connected to the dark portion observed in the first liquid crystal layer. The ratio of is calculated according to the following formula. The value obtained by arithmetically averaging the measured values is taken as the connection rate of the dark part.
- the dark portion observed in the second liquid crystal layer is preferably inclined with respect to the main surface of the second liquid crystal layer.
- first cholesteric liquid crystal layer for example, the degree of circular polarization of the light reflected by the reflecting surface derived from the cholesteric liquid crystal is increased.
- the dark portion observed in the first liquid crystal layer is inclined with respect to the main surface of the first liquid crystal layer and is observed in the second liquid crystal layer. It is more preferable that the dark portion to be formed is inclined with respect to the main surface of the second liquid crystal layer.
- the inclination direction of the dark portion observed in the second liquid crystal layer is preferably the same as the inclination direction of the dark portion observed in the first liquid crystal layer.
- the tilting direction of the dark portion observed in the second liquid crystal layer is the same as the tilting direction of the dark portion observed in the first liquid crystal layer.
- the angle formed by the straight line (virtual line) and the straight line (virtual line) passing through both ends of the dark portion observed in the second liquid crystal layer in the longitudinal direction is in the range of 100 ° to 180 °.
- the angle formed by the two straight lines is preferably in the range of 120 ° to 180 °, and more preferably in the range of 150 ° to 180 °.
- the dark portion observed in the second liquid crystal layer is inclined with respect to the main surface of the second liquid crystal layer (hereinafter, referred to as "inclination of the dark portion" in this paragraph). May be observed in at least one cross-sectional view in the thickness direction of the liquid crystal layer. For example, even if the inclination of the dark portion is not observed in any one cross-sectional view, the inclination of the dark portion may be observed in the other cross-sectional view.
- the angle of the dark part observed in the second liquid crystal layer is not limited.
- the average angle of the dark portion observed in the second liquid crystal layer is 10 ° with respect to the main surface of the second liquid crystal layer from the viewpoint of the uniformity of the inclination angle of the spiral axis.
- the above is preferable, 20 ° or more is more preferable, and 30 ° or more is particularly preferable.
- the average angle of the dark portion observed in the second liquid crystal layer is preferably 90 ° or less with respect to the main surface of the second liquid crystal layer.
- the average angle of the dark part observed in the second liquid crystal layer is the average angle of the dark part observed in the first liquid crystal layer described in the above section "1st cholesteric liquid crystal layer". Measure by a method similar to the measurement method of.
- the average angle of the dark part observed in the second liquid crystal layer may be the same as the average angle of the dark part observed in the first liquid crystal layer, or the first liquid crystal layer. It may be different from the average angle of the dark part observed in.
- the width of the dark part observed in the second liquid crystal layer is not limited.
- the distance between two adjacent dark portions among the dark portions observed in the second liquid crystal layer is preferably 0.05 ⁇ m or more, more preferably 0.1 ⁇ m or more. It is particularly preferably 0.15 ⁇ m or more.
- the distance between two adjacent dark parts among the dark parts observed in the second liquid crystal layer is preferably 500 ⁇ m or less, more preferably 100 ⁇ m or less, and more preferably 15 ⁇ m or less. It is more preferably 5 ⁇ m or less, and particularly preferably 5 ⁇ m or less.
- the distance between two adjacent dark parts among the dark parts observed in the second liquid crystal layer is the method for measuring the distance between the dark parts described in the above section "First cholesteric liquid crystal layer”. Measure by the method according to.
- the distance between the two adjacent dark areas observed in the second liquid crystal layer is the same as the distance between the two adjacent dark areas observed in the first liquid crystal layer. It may be different from the distance between two adjacent dark parts in the dark part observed in the first liquid crystal layer.
- the distance between two adjacent dark parts among the dark parts observed in the second liquid crystal layer is the distance between the dark parts observed in the first liquid crystal layer from the viewpoint of improving the connection rate of the dark parts. It is preferable that the distance is different from the distance between two adjacent dark areas.
- the distance between the two adjacent dark parts of the dark part observed in the second liquid crystal layer is the distance between the two adjacent dark parts of the dark part observed in the first liquid crystal layer. It is preferably larger than the distance of.
- the ratio of the distance between the two adjacent dark parts of the dark part observed in the first liquid crystal layer to the distance of the two adjacent dark parts in the dark part observed in the second liquid crystal layer is From the viewpoint of improving the connection rate of the dark part, it is preferably 0.8 to 5, more preferably 0.9 to 3, and particularly preferably 1 to 2. Further, in the cross-sectional view in the thickness direction, the distance between the two adjacent dark parts of the dark part observed in the first liquid crystal layer is the distance between the two adjacent dark parts of the dark part observed in the second liquid crystal layer.
- the ratio is preferably 1.1 to 2, more preferably 1.2 to 2, and particularly preferably 1.3 to 2.
- the liquid crystal compounds observed on the surface of the second liquid crystal layer opposite to the surface in contact with the first liquid crystal layer are arranged while being twisted along one of the in-plane directions of the second liquid crystal layer. It is preferable to have.
- the linearity of the dark part and the bright part observed in the cross section in the thickness direction becomes high, so that the haze of the cholesteric liquid crystal film can be further reduced.
- the thickness of the second liquid crystal layer is not limited.
- the average thickness of the second liquid crystal layer is 0.1 ⁇ m or more from the viewpoint of suppressing the influence of the smoothness of the surface shape of the layer adjacent to the second liquid crystal layer (for example, the first liquid crystal layer). It is preferably 0.5 ⁇ m or more, more preferably 1 ⁇ m or more, and particularly preferably 1 ⁇ m or more. From the viewpoint of transparency, the average thickness of the second liquid crystal layer is preferably 500 ⁇ m or less, more preferably 100 ⁇ m or less, and particularly preferably 20 ⁇ m or less.
- the average thickness of the second liquid crystal layer is measured by a method according to the method for measuring the average thickness of the first liquid crystal layer described in the above section "First cholesteric liquid crystal layer”.
- the thickness of the second liquid crystal layer may be the same as the thickness of the first liquid crystal layer, or may be different from the thickness of the first liquid crystal layer.
- the ratio of the thickness of the second liquid crystal layer to the thickness of the first liquid crystal layer is preferably 0.1 to 10, more preferably 0.2 to 5, and 0.3 to 3. It is particularly preferable to have.
- composition of the second liquid crystal layer is not limited as long as a striped pattern in which dark areas and bright areas are alternately arranged is observed.
- components of the second liquid crystal layer will be specifically described.
- the second liquid crystal layer preferably contains a liquid crystal compound.
- the liquid crystal compound include the liquid crystal compounds described in the above section "First cholesteric liquid crystal layer".
- the preferred embodiment of the liquid crystal compound is the same as the preferred embodiment of the liquid crystal compound described in the above section "First cholesteric liquid crystal layer”.
- the second liquid crystal layer may contain one kind alone or two or more kinds of liquid crystal compounds.
- the content of the liquid crystal compound in the second liquid crystal layer is preferably 70% by mass or more, and preferably 80% by mass or more, based on the total mass of the second liquid crystal layer. It is more preferably 90% by mass or more, and particularly preferably 90% by mass or more.
- the upper limit of the content of the liquid crystal compound is not limited.
- the content of the liquid crystal compound in the second liquid crystal layer may be determined in the range of 100% by mass or less with respect to the total mass of the second liquid crystal layer.
- the content of the liquid crystal compound in the second liquid crystal layer is less than 100% by mass and 99% by mass with respect to the total mass of the second liquid crystal layer. It may be less than or equal to 96% by mass or less.
- the second liquid crystal layer may contain components other than the liquid crystal compound (hereinafter, referred to as "other components" in this paragraph).
- Other components include, for example, chiral agents, solvents, orientation regulators, polymerization initiators, leveling agents, orientation aids, and sensitizers.
- the components of the cholesteric liquid crystal film according to the present disclosure are not limited as long as the first liquid crystal layer and the second liquid crystal layer are included.
- the cholesteric liquid crystal film according to the present disclosure may have components other than the first liquid crystal layer and the second liquid crystal layer.
- the cholesteric liquid crystal film according to the present disclosure may have a cholesteric liquid crystal layer other than the first liquid crystal layer and the second liquid crystal layer (hereinafter, referred to as "another cholesteric liquid crystal layer”), if necessary. good.
- the cholesteric liquid crystal film according to the present disclosure may have three or more cholesteric liquid crystal layers including a first liquid crystal layer and a second liquid crystal layer.
- the mode of the other cholesteric liquid crystal layer is limited. Not done.
- a preferred embodiment of the other cholesteric liquid crystal layer is the first liquid crystal layer described in the above-mentioned "first cholesteric liquid crystal layer” section, or the second liquid crystal layer described in the above-mentioned "second cholesteric liquid crystal layer” section. It is the same as the preferable aspect of.
- the combination of the first liquid crystal layer and the cholesteric liquid crystal layer corresponding to the second liquid crystal layer may be plural.
- the first cholesteric liquid crystal layer and the second cholesteric liquid crystal layer are formed on the first liquid crystal layer and the second liquid crystal layer.
- the second cholesteric liquid crystal layer and the third cholesteric liquid crystal layer may correspond to the first liquid crystal layer and the second liquid crystal layer, respectively.
- the cholesteric liquid crystal film has three or more cholesteric liquid crystal layers, it is preferable that all the cholesteric liquid crystal layers are stacked.
- the cholesteric liquid crystal film according to the present disclosure may have a base material. According to the base material, the strength of the cholesteric liquid crystal film can be improved.
- the base material may be arranged on the surface of the first liquid crystal layer opposite to the surface in contact with the second liquid crystal layer.
- the base material may be arranged on the surface of the second liquid crystal layer opposite to the surface in contact with the first liquid crystal layer.
- the cholesteric liquid crystal film according to the present disclosure preferably has a base material, a first liquid crystal layer, and a second liquid crystal layer in this order.
- the total light transmittance of the base material is preferably 80% or more, more preferably 85% or more, and particularly preferably 90% or more.
- the upper limit of the total light transmittance of the base material is not limited.
- the total light transmittance of the base material may be determined, for example, in the range of 100% or less.
- the total light transmittance of the base material is measured using a known spectrophotometer (for example, haze meter NDH 2000, Nippon Denshoku Industries Co., Ltd.).
- the base material is preferably a base material containing a polymer.
- the base material containing the polymer include a polyester-based base material (for example, polyethylene terephthalate and polyethylene naphthalate), a cellulose-based base material (for example, diacetyl cellulose and triacetyl cellulose (abbreviation: TAC)), and a polycarbonate-based base material.
- Substrate poly (meth) acrylic substrate (eg, poly (meth) acrylate (eg, polymethylmethacrylate)), polystyrene-based substrate (eg, polystyrene and acrylonitrile styrene copolymer), olefin-based substrate (eg, olefin-based substrate (eg, polystyrene and acrylonitrile styrene copolymer)
- polyamide-based substrates eg, polyvinyl chloride, nylon, and aromatic polyamides
- polyimide-based substrates Polysulfone-based base material, polyethersulfone-based base material, polyether etherketone-based base material, polyphenylene sulfide-based base material, vinyl alcohol-based base material, polyvinylid
- the shape of the base material is not limited.
- the shape of the base material may be determined, for example, according to the application and the installation location.
- the base material is preferably a flat base material.
- the thickness of the base material is preferably in the range of 30 ⁇ m to 250 ⁇ m, more preferably in the range of 40 ⁇ m to 100 ⁇ m, from the viewpoint of manufacturing suitability, manufacturing cost, and optical characteristics.
- the cholesteric liquid crystal film according to the present disclosure may have an orientation layer. According to the alignment layer, an orientation regulating force can be given to the liquid crystal compound.
- the alignment layer is preferably arranged between the base material and the cholesteric liquid crystal layer (preferably the first liquid crystal layer or the second liquid crystal layer).
- the cholesteric liquid crystal film according to the present disclosure preferably has a base material, an alignment layer, a first liquid crystal layer, and a second liquid crystal layer in this order.
- the alignment layer for example, a known alignment layer having a function of imparting an orientation regulating force to the liquid crystal compound can be used.
- the alignment layer may be an alignment layer in which an alignment function is generated by applying an electric field, applying a magnetic field, or irradiating light.
- the thickness of the alignment layer is preferably in the range of 0.1 ⁇ m to 10 ⁇ m, and more preferably in the range of 1 ⁇ m to 5 ⁇ m.
- the shape of the cholesteric liquid crystal film according to the present disclosure is not limited.
- Examples of the shape of the cholesteric liquid crystal film in a plan view include a circle (for example, a perfect circle and an ellipse), a polygon (for example, a triangle, a quadrangle, a pentagon, and a hexagon), and an indefinite shape.
- the thickness of the cholesteric liquid crystal film according to the present disclosure is not limited.
- the thickness of the cholesteric liquid crystal film according to the present disclosure is preferably in the range of 1 ⁇ m to 500 ⁇ m, more preferably in the range of 2 ⁇ m to 250 ⁇ m, and particularly preferably in the range of 5 ⁇ m to 100 ⁇ m.
- the use of the cholesteric liquid crystal film according to the present disclosure is not limited.
- Examples of the use of the cholesteric liquid crystal film according to the present disclosure include an optical film.
- the cholesteric liquid crystal film according to the present disclosure may be used, for example, as an optical film used for an aerial imaging device, a transparent screen, or an optical sensor member.
- the method for producing a cholesteric liquid crystal film according to the present disclosure includes a step of applying a first composition containing a liquid crystal compound and a chiral agent on a substrate (hereinafter, may be referred to as “step (A1)”).
- a step of applying a shearing force to the surface of the first composition applied on the substrate (hereinafter, may be referred to as “step (B1)”) and the first step of applying the shearing force.
- a step of forming the first cholesteric liquid crystal layer by curing the composition hereinafter, may be referred to as “step (C1)”), and a liquid crystal compound and chiral on the first cholesteric liquid crystal layer.
- step (A2) The step of applying the second composition containing the agent (hereinafter, may be referred to as “step (A2)”) and the surface of the second composition applied on the first cholesteric liquid crystal layer.
- step (B2) A step of applying a shearing force (hereinafter, may be referred to as “step (B2)”) and a step of forming a second cholesteric liquid crystal layer by curing the second composition to which the shearing force is applied. (Hereinafter, it may be referred to as “step (C2)").
- step (C2) a step of cholesteric liquid crystal film having a small haze can be manufactured.
- the first composition and the second composition may be collectively referred to as "composition”. ..
- coating the first composition on a base material is not limited to bringing the first composition into direct contact with the base material, and the first is applied to the base material via an arbitrary layer. Includes contacting the compositions. Any layer may be one of the constituents of the substrate, or it may be a layer formed on the substrate prior to application of the composition. As the arbitrary layer, for example, the orientation layer described in the above-mentioned "Orientation layer” section can be mentioned. The method of forming the oriented layer will be described later.
- the base material examples include the base materials described in the above section “Base material”.
- Preferred embodiments of the substrate eg, total light transmittance, type, shape, and thickness
- An alignment layer may be arranged in advance on the surface of the base material. When the alignment layer is arranged on the surface of the substrate, the first composition is applied on the alignment layer.
- liquid crystal compound for example, the liquid crystal compound described in the above section "First cholesteric liquid crystal layer” can be used.
- the preferred embodiment of the liquid crystal compound is the same as the preferred embodiment of the liquid crystal compound described in the above section "First cholesteric liquid crystal layer”.
- the first composition may contain one kind alone or two or more kinds of liquid crystal compounds.
- the content of the liquid crystal compound in the first composition is preferably 70% by mass or more, preferably 80% by mass or more, based on the solid content mass of the first composition. Is more preferable, and 90% by mass or more is particularly preferable.
- the upper limit of the content of the liquid crystal compound is not limited.
- the content of the liquid crystal compound in the first composition may be less than 100% by mass, 99% by mass or less, or 96% by mass or less with respect to the solid content mass of the first composition.
- chiral agent The type of chiral auxiliary is not limited.
- the chiral agent include known chiral agents (for example, "Liquid Crystal Device Handbook, Chapter 3, Section 4-3, Chiral Auxiliary for TN, STN, p. 199, Japan Society for the Promotion of Science, 42nd Committee, 1989".
- the chiral agent described in 1) can be used.
- chiral agents contain asymmetric carbon atoms.
- the chiral agent is not limited to compounds containing an asymmetric carbon atom.
- examples of the chiral agent include an axial asymmetric compound containing no asymmetric carbon atom and a plane asymmetric compound.
- Examples of the axial asymmetric compound or the planar asymmetric compound include binaphthyl, helicene, paracyclophane, and derivatives thereof.
- the chiral agent may have a polymerizable group.
- a chiral agent having a polymerizable group by reacting a chiral agent having a polymerizable group with a liquid crystal compound having a polymerizable group, a polymer having a structural unit derived from the chiral agent and a structural unit derived from the liquid crystal compound can be obtained.
- Examples of the polymerizable group in the chiral agent include the polymerizable group described in the above section "Liquid crystal compound".
- the preferred embodiment of the polymerizable group in the chiral agent is the same as the preferred embodiment of the polymerizable group described in the above section “Liquid crystal compound”.
- the type of polymerizable group in the chiral agent is preferably the same as the type of polymerizable group in the liquid crystal compound.
- Examples of the chiral agent exhibiting a strong twisting force include JP-A-2010-181852, JP-A-2003-287623, JP-A-2002-80851, JP-A-2002-80478, or JP-A-2002-302487. Examples thereof include chiral agents described in Japanese Patent Publication No.
- isosorbide compounds having a corresponding structure can also be used as a chiral agent.
- isosorbide compounds having a corresponding structure can also be used as a chiral agent.
- the first composition may contain one kind alone or two or more kinds of chiral agents.
- the content of the chiral agent is preferably 0.1% by mass to 20.0% by mass, preferably 0.2% by mass to 15.0% by mass, based on the solid content mass of the first composition. It is more preferable, and it is particularly preferable that it is 0.5% by mass to 10.0% by mass.
- the first composition may contain components other than the above-mentioned components (hereinafter, referred to as "other components” in this paragraph).
- Other components include, for example, solvents, orientation regulators, polymerization initiators, leveling agents, orientation aids, and sensitizers.
- an organic solvent is preferable.
- the organic solvent include an amide solvent (for example, N, N-dimethylformamide), a sulfoxide solvent (for example, dimethyl sulfoxide), a heterocyclic compound (for example, pyridine), a hydrocarbon solvent (for example, benzene, and hexane), and the like.
- Alkyl halide solvents eg chloroform, dichloromethane
- ester solvents eg methyl acetate and butyl acetate
- ketone solvents eg acetone, methyl ethyl ketone, and cyclohexanone
- ether solvents eg tetrahydrofuran, and 1, 2 -Dimethoxyethane.
- the organic solvent is preferably at least one selected from the group consisting of an alkyl halide solvent and a ketone solvent, and more preferably a ketone solvent.
- the first composition may contain one kind alone or two or more kinds of solvents.
- the content of the solid content in the first composition is preferably 25% by mass to 40% by mass, and preferably 25% by mass to 35% by mass, based on the total mass of the first composition. More preferred.
- orientation control agent examples include the compounds described in paragraphs [0012] to [0030] of JP2012-2011306A, and paragraphs [0037] to [0044] of JP2012-101999.
- Examples include compounds.
- a polymer containing the polymerization unit of the fluoroaliphatic group-containing monomer in an amount of more than 50% by mass of the total polymerization unit described in JP-A-2004-331812 may be used as the orientation control agent.
- a vertical alignment agent can also be mentioned as an orientation control agent.
- Examples of the vertical alignment agent include a boronic acid compound and / or an onium salt described in JP-A-2015-38598, and an onium salt described in JP-A-2008-26730.
- the content of the orientation control agent is more than 0% by mass and 5.0% by mass or less with respect to the solid content mass of the first composition. It is preferably, and more preferably 0.3% by mass to 2.0% by mass.
- polymerization initiator examples include a photopolymerization initiator and a thermal polymerization initiator.
- the polymerization initiator is preferably a photopolymerization initiator from the viewpoint of suppressing deformation of the base material due to heat and deterioration of the first composition.
- the photopolymerization initiator include an ⁇ -carbonyl compound (for example, the compound described in US Pat. No. 2,376,661 or US Pat. No. 2,376,670) and an acyloin ether (for example, US Pat. No. 2,448,828).
- ⁇ -carbonyl compound for example, the compound described in US Pat. No. 2,376,661 or US Pat. No. 2,376,670
- an acyloin ether for example, US Pat. No. 2,448,828.
- Compounds described in the specification ⁇ -hydrogen-substituted aromatic acidoine compounds (eg, compounds described in US Pat. No. 2,725,212), polynuclear quinone compounds (eg, US Pat. No. 3,46127, or US Pat.
- Kaisho 60-105667 or a compound described in US Pat. No. 4,239,850
- a phenazine compound for example, JP-A-60-105667, or a compound described in US Pat. No. 4,239,850
- Oxaziazole compounds for example, the compounds described in US Pat. No. 4,212,970
- acylphosphine oxide compounds for example, Japanese Patent Application Laid-Open No. 63-40799, Japanese Patent Application Laid-Open No. 5-29234, JP-A-10- Examples thereof include compounds described in Japanese Patent Application Laid-Open No. 95788 or JP-A-10-29997).
- the content of the polymerization initiator is 0.5% by mass to 5.0% by mass with respect to the solid content mass of the first composition. It is preferable, and it is more preferable that it is 1.0% by mass to 4.0% by mass.
- the method for producing the first composition is not limited.
- Examples of the method for producing the first composition include a method of mixing the above components.
- As the mixing method a known mixing method can be used.
- the obtained mixture may be filtered.
- the method of applying the first composition is not limited.
- the coating method of the first composition include an extrusion die coater method, a curtain coating method, a dip coating method, a spin coating method, a print coating method, a spray coating method, a slot coating method, a roll coating method, and a slide coating method.
- Examples include a blade coating method, a gravure coating method, and a wire bar method.
- the amount of the first composition applied is not limited.
- the coating amount of the first composition is, for example, the thickness of the target cholesteric liquid crystal layer or the thickness of the first composition before the shearing force described in the section "Step (B1)" below is applied. It may be decided according to.
- -Means to apply shear force- Means for applying shear force include, for example, blades, air knives, bars, and applicators.
- the thickness of the first composition may change before and after applying the shearing force.
- the thickness of the first composition after the shearing force is applied by the blade is 1/2 or less, or 1/3 or less, of the thickness of the first composition before the shearing force is applied. There may be.
- the thickness of the first composition after the shearing force is applied by the blade is preferably 1/4 or more with respect to the thickness of the first composition before the shearing force is applied.
- the material of the blade is not limited.
- the blade material include metals (eg, stainless steel) and resins (eg, Teflon® and polyetheretherketone (PEEK)).
- the shape of the blade is not limited. Examples of the shape of the blade include a plate shape.
- the blade is preferably a metal plate-shaped member from the viewpoint that a shearing force is easily applied to the first composition.
- the thickness of the tip of the blade in contact with the first composition is preferably 0.1 mm or more, and preferably 1 mm or more, from the viewpoint of easily applying a shearing force to the first composition. More preferred. There is no upper limit to the thickness of the blade. The thickness of the blade may be determined in the range of, for example, 10 mm or less.
- the shearing force is applied to the surface of the first composition by blowing compressed air on the surface of the first composition with an air knife.
- the shear rate applied to the first composition can be adjusted according to the rate at which the compressed air is blown (that is, the flow velocity).
- the direction in which the compressed air is blown by the air knife may be the same direction or the opposite direction to the transport direction of the first composition.
- the blowing direction of the compressed air by the air knife is a first composition from the viewpoint of preventing fragments of the first composition scraped by the compressed air from adhering to the first composition remaining on the substrate. It is preferable that the direction is the same as the transport direction of.
- the shear rate in the step (B1) the higher the orientation accuracy of the cholesteric liquid crystal layer can be formed.
- the shear rate is preferably 1,000 seconds-1 or more, more preferably 10,000 seconds- 1 or more, and particularly preferably 30,000 seconds-1 or more.
- the upper limit of shear rate is not limited. Shear rate, for example, may be determined in the range of 1.0 ⁇ 10 6 sec -1 or less.
- the shear rate is such that the shortest distance between the blade and the base material is "d", and the transfer rate of the first composition in contact with the blade (that is, the first composition).
- the relative speed between the blade and the blade is "V”
- the shear rate is the relative speed between the surface of the first composition and the surface of the base material, where the thickness of the first composition after the application of shear is "h”.
- V it is obtained by "V / 2h".
- the surface temperature of the first composition when a shearing force is applied may be determined according to the phase transition temperature of the liquid crystal compound contained in the first composition.
- the surface temperature of the first composition when a shearing force is applied is preferably 50 ° C. to 120 ° C., more preferably 60 ° C. to 100 ° C.
- the surface temperature of the first composition is measured using a radiation thermometer whose emissivity is calibrated by the temperature value measured by a non-contact thermometer.
- the surface temperature of the first composition is measured within 10 cm from the surface on the side opposite to the measurement surface (that is, the back side) in the absence of reflectors.
- the thickness of the first composition before the shearing force is applied is preferably in the range of 30 ⁇ m or less, preferably in the range of 15 ⁇ m to 25 ⁇ m, from the viewpoint of forming a cholesteric liquid crystal layer having high orientation accuracy. More preferred.
- the thickness of the first composition after the shearing force is applied is preferably in the range of 10 ⁇ m or less, and preferably in the range of 7 ⁇ m or less, from the viewpoint of forming a cholesteric liquid crystal layer having high orientation accuracy. More preferred.
- the lower limit of the thickness of the first composition after the shear force is applied is not limited.
- the thickness of the first composition after the shearing force is applied is preferably in the range of 5 ⁇ m or more.
- the first cholesteric liquid crystal layer is formed by curing the first composition to which the shearing force is applied.
- Examples of the method for curing the first composition include heating and irradiation with active energy rays.
- the step (C1) from the viewpoint of production suitability, it is preferable to cure the composition by applying a shearing force and irradiating the first composition with active energy rays.
- active energy rays examples include ⁇ -rays, ⁇ -rays, X-rays, ultraviolet rays, infrared rays, visible rays, and electron beams.
- the active energy ray is preferably ultraviolet rays from the viewpoint of curing sensitivity and availability of the apparatus.
- Light sources of ultraviolet rays include, for example, lamps (eg, tungsten lamps, halogen lamps, xenon lamps, xenon flash lamps, mercury lamps, mercury xenon lamps, and carbon arc lamps), lasers (eg, semiconductor lasers, helium neon lasers, argons). Examples thereof include an ion laser, a helium cadmium laser, and a YAG (Ytrium Aluminum Garnet) laser, a light emitting diode, and a cathode line tube.
- lamps eg, tungsten lamps, halogen lamps, xenon lamps, xenon flash lamps, mercury lamps, mercury xenon lamps, and carbon arc lamps
- lasers eg, semiconductor lasers, helium neon lasers, argons. Examples thereof include an ion laser, a helium cadmium laser, and a YAG (Ytrium Aluminum Garnet) laser, a light emitting diode, and a cathode
- the peak wavelength of ultraviolet rays emitted from the light source of ultraviolet rays is preferably 200 nm to 400 nm.
- the exposure amount of ultraviolet rays (also referred to as integrated light amount) is preferably 100 mJ / cm 2 to 500 mJ / cm 2.
- a second composition containing a liquid crystal compound and a chiral agent is applied onto the first cholesteric liquid crystal layer.
- process (A1) The items described in the above "process (A1)" section (excluding items related to the base material) are applied to the process (A2).
- the preferred embodiment of the step (A2) is the same as the preferred embodiment of the step (A1).
- process (B1) The matters described in the above "process (B1)" section are applied to the process (B2).
- the preferred embodiment of the step (B2) is the same as the preferred embodiment of the step (B1).
- the second cholesteric liquid crystal layer is formed by curing the second composition to which the shearing force is applied.
- process (C1) The matters described in the above "process (C1)" section are applied to the process (C2).
- the preferred embodiment of the step (C2) is the same as the preferred embodiment of the step (C1).
- the method for producing a cholesteric liquid crystal film according to the present disclosure may include steps other than the above-mentioned steps.
- the method for producing a cholesteric liquid crystal film according to the present disclosure may include, for example, a step of forming an alignment layer on a substrate (hereinafter, may be referred to as “step (D)”).
- step (D) is preferably carried out before the step (A1).
- Examples of the method for forming the oriented layer include rubbing treatment of an organic compound (preferably a polymer), oblique vapor deposition of an inorganic compound, and formation of a layer having microgrooves.
- the method for producing a cholesteric liquid crystal film according to the present disclosure determines the content of the solvent in the composition with respect to the total mass of the composition before applying a shearing force to the surface of the composition. It is preferable to have a step of adjusting to a range of 50% by mass or less (hereinafter, may be referred to as "step (E)"). Specifically, in the method for producing a cholesteric liquid crystal film according to the present disclosure, the content of the solvent in the first composition applied on the substrate is described above between the step (A1) and the step (B1).
- a step of adjusting the composition it is preferable to have a step of adjusting the composition to a range of 50% by mass or less with respect to the total mass of the composition.
- the content of the solvent in the second composition coated on the first cholesteric liquid crystal layer between the steps (A2) and the step (B2) is described above. It is preferable to have a step of adjusting the composition to a range of 50% by mass or less with respect to the total mass of the composition.
- the step (E) may be carried out between the step (A1) and the step (B1), or between the step (A2) and the step (B2).
- the step (E) may be carried out between the step (A1) and the step (B1), and between the step (A2) and the step (B2).
- the content of the solvent in the composition is preferably 40% by mass or less, more preferably 30% by mass or less, based on the total mass of the composition.
- the lower limit of the solvent content in the composition is not limited.
- the content of the solvent in the composition may be 0% by mass or may exceed 0% by mass with respect to the total mass of the composition.
- the content of the solvent in the composition is preferably 10% by mass or more from the viewpoint of easily suppressing deterioration of the surface state of the composition.
- the content of the solvent in the composition is measured by the absolute drying method.
- the sample collected from the composition is dried at 60 ° C. for 24 hours, and then the mass change of the sample before and after drying (that is, the difference between the mass of the sample after drying and the mass of the sample before drying) is determined.
- the arithmetic mean of the values obtained by performing the above operation three times is taken as the solvent content.
- step (E) as a method for adjusting the content of the solvent in the composition, for example, drying can be mentioned.
- Drying means include, for example, ovens, hot air blowers, and infrared (IR) heaters.
- warm air may be directly applied to the composition, or warm air may be applied to the surface opposite to the surface on which the composition of the base material is arranged. Further, a diffusion plate may be installed in order to prevent the surface of the composition from flowing due to warm air.
- Drying may be done by inhalation.
- a decompression chamber having an exhaust mechanism can be used. By inhaling the gas around the composition, the content of the solvent in the composition can be reduced.
- the drying conditions are not limited as long as the content of the solvent in the composition can be adjusted in the range of 50% by mass or less.
- the drying conditions may be determined, for example, according to the components contained in the composition, the coating amount of the composition, and the transport speed.
- the method for producing a cholesteric liquid crystal film according to the present disclosure may be carried out by a roll-to-roll method.
- each step is carried out while continuously transporting a long base material.
- the method for producing a cholesteric liquid crystal film according to the present disclosure may be carried out using a base material that is conveyed one by one.
- the cholesteric liquid crystal film of Example 1 was produced by the following procedure.
- the cholesteric liquid crystal film of Example 1 has a base material, an alignment layer, a first cholesteric liquid crystal layer, and a second cholesteric liquid crystal layer in this order.
- a triacetyl cellulose (TAC) film (FUJIFILM Corporation, refractive index: 1.48, thickness: 40 ⁇ m) was prepared.
- the composition for forming an orientation layer is prepared by stirring a mixture containing pure water (96 parts by mass) and PVA-205 (4 parts by mass, Kuraray Co., Ltd., polyvinyl alcohol) in a container kept warm at 80 ° C. Prepared. Using a bar (bar count: 6), the composition for forming an orientation layer was applied onto a substrate (triacetyl cellulose film), and then dried in an oven at 100 ° C. for 10 minutes. By the above procedure, an orientation layer (thickness: 2 ⁇ m) was formed on the base material.
- a first cholesteric liquid crystal layer (thickness: 8 ⁇ m) was formed on the oriented layer by the following procedure.
- a coating liquid (1) for forming a liquid crystal layer was prepared by filtering using a polypropylene filter (pore diameter: 0.2 ⁇ m).
- Rod-shaped thermotropic liquid crystal compound (compound (A) below): 100 parts by mass (2) Chiral agent (compound (B) below, Palicol® LC756, BASF): 1.7 parts by mass (3) Photopolymerization initiator (IRGACURE (registered trademark) 907, BASF): 3 parts by mass (4) Photopolymerization initiator (PM758, Nippon Kayaku Co., Ltd.): 1 part by mass (5) Orientation regulator (the following compound (C) )): 0.5 parts by mass (6) Solvent (methyl ethyl ketone): 184 parts by mass (7) Solvent (cyclohexanone): 31 parts by mass
- Compound (A) is a mixture of the following three compounds.
- the content of each compound in the mixture is 84% by mass, 14% by mass, and 2% by mass in this order from the top.
- the base material having the alignment layer was heated at 70 ° C., and then the liquid crystal layer forming coating liquid (1) was applied onto the alignment layer using a bar (bar number: 18).
- the liquid crystal layer forming coating liquid (1) coated on the alignment layer is dried in an oven at 70 ° C. for 1 minute to form a coating film (thickness: 10 ⁇ m, solvent content: 1% by mass or less). Formed.
- the coating film to which the shearing force was applied was irradiated with ultraviolet rays (exposure amount: 500 mJ / cm 2 ) using a metal halide lamp to cure the coating film.
- a second cholesteric liquid crystal layer (thickness: 8 ⁇ m) was formed on the first cholesteric liquid crystal layer by the following procedure.
- a coating liquid (2) for forming a liquid crystal layer was prepared by filtering using a polypropylene filter (pore diameter: 0.2 ⁇ m).
- Rod-shaped thermotropic liquid crystal compound (Compound (A)): 100 parts by mass (2) Chiral agent (Compound (B), Policolor (registered trademark) LC756, BASF): 1.2 parts by mass (3) Photopolymerization Initiator (IRGACURE® 907, BASF): 1 part by mass (4) Photopolymerization initiator (PM758, Nippon Kayaku Co., Ltd.): 1 part by mass (5) Orientation control agent (Compound (C)): 0.5 parts by mass (6) Solvent (methyl ethyl ketone): 184 parts by mass (7) Solvent (cyclohexanone): 31 parts by mass
- the base material having the first cholesteric liquid crystal layer is heated at 70 ° C., and then the liquid crystal layer forming coating liquid (2) is applied onto the first cholesteric liquid crystal layer using a bar (bar count: 18). It was applied.
- the liquid crystal layer forming coating liquid (2) coated on the first cholesteric liquid crystal layer is dried in an oven at 70 ° C. for 1 minute to obtain a coating film (thickness: 10 ⁇ m, solvent content: 1 mass). % Or less) was formed.
- the coating film to which the shearing force was applied was irradiated with ultraviolet rays (exposure amount: 500 mJ / cm 2 ) using a metal halide lamp to cure the coating film.
- Example 2 The cholesteric liquid crystal film of Example 2 was produced by the same procedure as in Example 1 except that the amount of the chiral agent added in the liquid crystal layer forming coating liquid (1) was changed to 1.2 parts by mass.
- the cross section of the cholesteric liquid crystal film of Example 2 in the thickness direction was observed by the same procedure as in Example 1.
- a striped pattern in which dark areas and bright areas were alternately arranged was observed.
- the dark portion observed in the second cholesteric liquid crystal layer was connected to the dark portion observed in the first cholesteric liquid crystal layer.
- the cross section of the cholesteric liquid crystal film of Comparative Example 1 in the thickness direction was observed by the same procedure as in Example 1.
- the directions of the spiral axes in the second cholesteric liquid crystal layer are different, and the dark portion observed in the second cholesteric liquid crystal layer at the interface between the first cholesteric liquid crystal layer and the second cholesteric liquid crystal layer is the above-mentioned second cholesteric liquid crystal layer. It was not connected to the dark part observed in the cholesteric liquid crystal layer of 1.
- Table 1 shows that the haze of Examples 1 and 2 is smaller than the haze of Comparative Example 1.
Abstract
Description
本開示の一態様は、ヘイズが小さいコレステリック液晶膜を提供することを目的とする。
<1> 顕微鏡を用いて観察される暗部及び明部が交互に並んだ縞模様を有する第1のコレステリック液晶層と、上記第1のコレステリック液晶層に接して配置され、顕微鏡を用いて観察される暗部及び明部が交互に並んだ縞模様を有する第2のコレステリック液晶層と、を有し、上記第1のコレステリック液晶層と上記第2のコレステリック液晶層との界面において、上記第2のコレステリック液晶層で観察される上記暗部が、上記第1のコレステリック液晶層で観察される上記暗部に接続しているコレステリック液晶膜。
<2> 厚さ方向の断面視において、上記第2のコレステリック液晶層で観察される上記暗部のうち隣り合う2つの暗部の距離が、上記第1のコレステリック液晶層で観察される上記暗部のうち隣り合う2つの暗部の距離と異なる<1>に記載のコレステリック液晶膜。
<3> 厚さ方向の断面視において、上記第2のコレステリック液晶層で観察される上記暗部のうち隣り合う2つの暗部の距離が、上記第1のコレステリック液晶層で観察される上記暗部のうち隣り合う2つの暗部の距離よりも大きい<1>又は<2>に記載のコレステリック液晶膜。
<4> 厚さ方向の断面視において、上記第1のコレステリック液晶層で観察される上記暗部のうち隣り合う2つの暗部の距離に対する上記第2のコレステリック液晶層で観察される上記暗部のうち隣り合う2つの暗部の距離の比が、1~2である<1>に記載のコレステリック液晶膜。
<5> 厚さ方向の断面視において、上記第1のコレステリック液晶層で観察される上記暗部のうち隣り合う2つの暗部の距離が、0.1μm~2μmである<1>~<4>のいずれか1つに記載のコレステリック液晶膜。
<6> 厚さ方向の断面視において、上記第2のコレステリック液晶層で観察される上記暗部のうち隣り合う2つの暗部の距離が、0.1μm~5μmである<1>~<5>のいずれか1つに記載のコレステリック液晶膜。
<7> 上記第1のコレステリック液晶層と上記第2のコレステリック液晶層との界面において、上記第1のコレステリック液晶層で観察される上記暗部に接続している上記第2のコレステリック液晶層で観察される上記暗部の割合が、上記第2のコレステリック液晶層で観察される上記暗部の数に対して、50%~100%である<1>~<6>のいずれか1つに記載のコレステリック液晶膜。
<8> 厚さ方向の断面視において、上記第1のコレステリック液晶層で観察される上記暗部が、上記第1のコレステリック液晶層の主面に対して傾斜しており、かつ、上記第2のコレステリック液晶層で観察される上記暗部が、上記第2のコレステリック液晶層の主面に対して傾斜している<1>~<7>のいずれか1つに記載のコレステリック液晶膜。
<9> 厚さ方向の断面視において、上記第1のコレステリック液晶層で観察される上記暗部の平均角度が、上記第1のコレステリック液晶層の主面に対して、20°~90°である<1>~<8>のいずれか1つに記載のコレステリック液晶膜。
<10> 厚さ方向の断面視において、上記第2のコレステリック液晶層で観察される上記暗部の平均角度が、上記第2のコレステリック液晶層の主面に対して、30°~90°である<1>~<9>のいずれか1つに記載のコレステリック液晶膜。
<11> 上記第1のコレステリック液晶層の上記縞模様が、少なくとも、上記第1のコレステリック液晶層の厚さ方向の断面で観察され、かつ、上記第2のコレステリック液晶層の上記縞模様が、少なくとも、上記第2のコレステリック液晶層の厚さ方向の断面で観察される<1>~<10>のいずれか1つに記載のコレステリック液晶膜。
本開示に係るコレステリック液晶膜は、顕微鏡を用いて観察される暗部及び明部が交互に並んだ縞模様を有する第1のコレステリック液晶層と、上記第1のコレステリック液晶層に接して配置され、顕微鏡を用いて観察される暗部及び明部が交互に並んだ縞模様を有する第2のコレステリック液晶層と、を有し、上記第1のコレステリック液晶層と上記第2のコレステリック液晶層との界面において、上記第2のコレステリック液晶層で観察される上記暗部が、上記第1のコレステリック液晶層で観察される上記暗部に接続している。上記した本開示の一態様によれば、ヘイズが小さいコレステリック液晶膜が提供される。
本開示に係るコレステリック液晶膜は、顕微鏡を用いて観察される暗部及び明部が交互に並んだ縞模様を有する第1のコレステリック液晶層を有する。
液晶の一形態として知られるコレステリック液晶は、複数の液晶化合物がらせん状に配列することによって形成されるらせん構造を有する。らせん構造における液晶化合物の分子軸の向きは、らせん軸に沿って変化している。このため、顕微鏡を用いてコレステリック液晶を観察すると、観察方向に対する液晶化合物の分子軸の向きに応じて、暗部(相対的に暗く見える領域をいう。以下同じ。)、及び明部(相対的に明るく見える領域をいう。以下同じ。)が観察される。本開示において、暗部、及び明部を観察するための顕微鏡としては、特に断りのない限り、走査型電子顕微鏡、又は偏光顕微鏡を用いる。
第1の液晶層の厚さは、制限されない。第1の液晶層の平均厚さは、第1の液晶層に隣接する層(例えば、基材、及び第2の液晶層)の表面形状の平滑性による影響を抑制するという観点から、0.1μm以上であることが好ましく、0.5μm以上であることがより好ましく、1μm以上であることが特に好ましい。第1の液晶層の平均厚さは、透明性の観点から、500μm以下であることが好ましく、100μm以下であることがより好ましく、20μm以下であることが特に好ましい。
第1の液晶層の組成は、暗部及び明部が交互に並んだ縞模様が観察される限り、制限されない。以下、第1の液晶層の成分について具体的に説明する。
第1の液晶層は、液晶化合物を含むことが好ましい。液晶化合物の種類は、制限されない。液晶化合物としては、例えば、コレステリック液晶を形成する公知の液晶化合物を利用することができる。
第1の液晶層は、液晶化合物以外の成分(以下、本段落において「他の成分」という。)を含んでいてもよい。他の成分としては、例えば、キラル剤、溶媒、配向規制剤、重合開始剤、レベリング剤、配向助剤、及び増感剤が挙げられる。
本開示に係るコレステリック液晶膜は、第1のコレステリック液晶層に接して配置され、顕微鏡を用いて観察される暗部及び明部が交互に並んだ縞模様を有する第2のコレステリック液晶層を有する。
第2の液晶層で縞模様が観察される原理は、上記「第1のコレステリック液晶層」の項において説明した原理と同様である。
第2の液晶層の厚さは、制限されない。第2の液晶層の平均厚さは、第2の液晶層に隣接する層(例えば、第1の液晶層)の表面形状の平滑性による影響を抑制するという観点から、0.1μm以上であることが好ましく、0.5μm以上であることがより好ましく、1μm以上であることが特に好ましい。第2の液晶層の平均厚さは、透明性の観点から、500μm以下であることが好ましく、100μm以下であることがより好ましく、20μm以下であることが特に好ましい。
第2の液晶層の組成は、暗部及び明部が交互に並んだ縞模様が観察される限り、制限されない。以下、第2の液晶層の成分について具体的に説明する。
第2の液晶層は、液晶化合物を含むことが好ましい。液晶化合物としては、例えば、上記「第1のコレステリック液晶層」の項において説明した液晶化合物が挙げられる。液晶化合物の好ましい態様は、上記「第1のコレステリック液晶層」の項において説明した液晶化合物の好ましい態様と同様である。
第2の液晶層は、液晶化合物以外の成分(以下、本段落において「他の成分」という。)を含んでいてもよい。他の成分としては、例えば、キラル剤、溶媒、配向規制剤、重合開始剤、レベリング剤、配向助剤、及び増感剤が挙げられる。
本開示に係るコレステリック液晶膜の構成要素は、第1の液晶層、及び第2の液晶層を含む限り、制限されない。本開示に係るコレステリック液晶膜は、第1の液晶層、及び第2の液晶層以外の構成要素を有していてもよい。
本開示に係るコレステリック液晶膜は、必要に応じて、第1の液晶層、及び第2の液晶層以外のコレステリック液晶層(以下、「他のコレステリック液晶層」という。)を有していてもよい。言い換えると、本開示に係るコレステリック液晶膜は、第1の液晶層、及び第2の液晶層を含む、3つ以上のコレステリック液晶層を有していてもよい。
本開示に係るコレステリック液晶膜は、基材を有していてもよい。基材によれば、コレステリック液晶膜の強度を向上させることができる。
本開示に係るコレステリック液晶膜は、配向層を有していてもよい。配向層によれば、液晶化合物に対して配向規制力を与えることができる。
本開示に係るコレステリック液晶膜の形状は、制限されない。平面視におけるコレステリック液晶膜の形状としては、例えば、円形(例えば、真円、及び楕円)、多角形(例えば、三角形、四角形、五角形、及び六角形)、及び不定形が挙げられる。
本開示に係るコレステリック液晶膜の厚さは、制限されない。本開示に係るコレステリック液晶膜の厚さは、1μm~500μmの範囲であることが好ましく、2μm~250μmの範囲であることがより好ましく、5μm~100μmの範囲であることが特に好ましい。
本開示に係るコレステリック液晶膜の用途は、制限されない。本開示に係るコレステリック液晶膜の用途としては、例えば、光学フィルムが挙げられる。本開示に係るコレステリック液晶膜は、例えば、空中結像装置、透明スクリーン、又は光学センサー部材に用いられる光学フィルムとして用いてもよい。
以下、本開示に係るコレステリック液晶膜の製造方法について説明する。ただし、本開示に係るコレステリック液晶膜の製造方法は、以下に説明する方法に制限されるものではない。
工程(A1)においては、基材上に、液晶化合物、及びキラル剤を含む第1の組成物を塗布する。
基材としては、例えば、上記「基材」の項において説明した基材が挙げられる。基材の好ましい態様(例えば、全光線透過率、種類、形状、及び厚さ)は、上記「基材」の項において説明した基材の好ましい態様と同様である。基材の表面に、予め配向層が配置されていてもよい。基材の表面に配向層が配置されている場合、第1の組成物は、配向層上に塗布される。
液晶化合物としては、例えば、上記「第1のコレステリック液晶層」の項において説明した液晶化合物を利用することができる。液晶化合物の好ましい態様は、上記「第1のコレステリック液晶層」の項において説明した液晶化合物の好ましい態様と同様である。
キラル剤の種類は、制限されない。キラル剤としては、例えば、公知のキラル剤(例えば、「液晶デバイスハンドブック、第3章4-3項、TN、STN用カイラル剤、199頁、日本学術振興会第一42委員会編、1989」に記載されたキラル剤)を利用することができる。
第1の組成物は、上記した成分以外の成分(以下、本段落において「他の成分」という。)を含んでいてもよい。他の成分としては、例えば、溶媒、配向規制剤、重合開始剤、レベリング剤、配向助剤、及び増感剤が挙げられる。
第1の組成物の製造方法は、制限されない。第1の組成物の製造方法としては、例えば、上記各成分を混合する方法が挙げられる。混合方法としては、公知の混合方法を利用することができる。第1の組成物の製造方法においては、上記各成分を混合した後、得られた混合物をろ過してもよい。
第1の組成物の塗布方法は、制限されない。第1の組成物の塗布方法としては、例えば、エクストルージョンダイコータ法、カーテンコーティング法、ディップコーティング法、スピンコーティング法、印刷コーティング法、スプレーコーティング法、スロットコーティング法、ロールコーティング法、スライドコーティング法、ブレードコーティング法、グラビアコーティング法、及びワイヤーバー法が挙げられる。
第1の組成物の塗布量は、制限されない。第1の組成物の塗布量は、例えば、目的とするコレステリック液晶層の厚さ、又は下記「工程(B1)」の項において説明するせん断力が与えられる前の第1の組成物の厚さに応じて決定すればよい。
工程(B1)においては、基材上に塗布された第1の組成物の表面にせん断力を与える。工程(B1)によれば、らせん軸の向きのばらつきを低減することができる。
せん断力を付与する手段としては、例えば、ブレード、エアナイフ、バー、及びアプリケーターが挙げられる。工程(B1)においては、ブレード、又はエアナイフを用いて組成物の表面にせん断力を与えることが好ましく、ブレードを用いて第1の組成物の表面にせん断力を与えることがより好ましい。
工程(B1)におけるせん断速度が大きいほど、配向精度が高いコレステリック液晶層を形成することができる。せん断速度は、1,000秒-1以上であることが好ましく、10,000秒-1以上であることがより好ましく、30,000秒-1以上であることが特に好ましい。せん断速度の上限は、制限されない。せん断速度は、例えば、1.0×106秒-1以下の範囲で決定すればよい。
せん断力が与えられる際の第1の組成物の表面温度は、第1の組成物に含まれる液晶化合物の相転移温度に応じて決定すればよい。せん断力が与えられる際の第1の組成物の表面温度は、50℃~120℃であることが好ましく、60℃~100℃であることがより好ましい。第1の組成物の表面温度を上記範囲に調整することで、配向精度が高いコレステリック液晶層を得ることができる。第1の組成物の表面温度は、非接触式温度計で測定した温度値によって放射率が校正された放射温度計を用いて測定する。第1の組成物の表面温度は、測定面とは反対側(すなわち、裏側)の表面から10cm以内に反射物がない状態で測定する。
せん断力が与えられる前の第1の組成物の厚さは、配向精度が高いコレステリック液晶層を形成するという観点から、30μm以下の範囲であることが好ましく、15μm~25μmの範囲であることがより好ましい。
工程(C1)においては、せん断力が与えられた第1の組成物を硬化させることによって第1のコレステリック液晶層を形成する。
工程(A2)においては、第1のコレステリック液晶層上に、液晶化合物、及びキラル剤を含む第2の組成物を塗布する。
工程(B2)においては、第1のコレステリック液晶層上に塗布された第2の組成物の表面にせん断力を与える。工程(B2)によれば、らせん軸の向きのばらつきを低減することができるため、暗部の接続率を向上させることができる。
工程(C2)においては、せん断力が与えられた第2の組成物を硬化させることによって第2のコレステリック液晶層を形成する。
本開示に係るコレステリック液晶膜の製造方法は、上記した工程以外の工程を有していてもよい。
本開示に係るコレステリック液晶膜の製造方法は、例えば、基材上に配向層を形成する工程(以下、「工程(D)」という場合がある。)を有していてもよい。工程(D)は、工程(A1)の前に実施されることが好ましい。
組成物が溶媒を含む場合、本開示に係るコレステリック液晶膜の製造方法は、組成物の表面にせん断力を与える前に、組成物中の溶媒の含有率を上記組成物の全質量に対して50質量%以下の範囲に調整する工程(以下、「工程(E)」という場合がある。)を有することが好ましい。具体的に、本開示に係るコレステリック液晶膜の製造方法は、工程(A1)と工程(B1)との間に、基材上に塗布された第1の組成物中の溶媒の含有率を上記組成物の全質量に対して50質量%以下の範囲に調整する工程を有することが好ましい。本開示に係るコレステリック液晶膜の製造方法は、工程(A2)と工程(B2)との間に、第1のコレステリック液晶層上に塗布された第2の組成物中の溶媒の含有率を上記組成物の全質量に対して50質量%以下の範囲に調整する工程を有することが好ましい。
本開示に係るコレステリック液晶膜の製造方法は、ロールトゥロール(Roll to Roll)方式によって実施してもよい。ロールトゥロール方式においては、例えば、長尺の基材を連続搬送しながら各工程を実施する。本開示に係るコレステリック液晶膜の製造方法は、1つずつ搬送される基材を用いて実施してもよい。
以下の手順によって、実施例1のコレステリック液晶膜を製造した。実施例1のコレステリック液晶膜は、基材と、配向層と、第1のコレステリック液晶層と、第2のコレステリック液晶層と、をこの順で有する。
基材として、トリアセチルセルロース(TAC)フィルム(富士フイルム株式会社、屈折率:1.48、厚さ:40μm)を用意した。
80℃で保温された容器中で、純水(96質量部)、及びPVA-205(4質量部、株式会社クラレ、ポリビニルアルコール)を含む混合物を撹拌することによって、配向層形成用組成物を調製した。バー(バーの番手:6)を用いて、基材(トリアセチルセルロースフィルム)上に上記配向層形成用組成物を塗布し、次いで、100℃のオーブン内で10分間乾燥した。以上の手順によって、基材の上に配向層(厚さ:2μm)を形成した。
以下の手順によって、配向層の上に第1のコレステリック液晶層(厚さ:8μm)を形成した。
下記に示す各成分を混合した後、ポリプロピレン製フィルター(孔径:0.2μm)を用いてろ過することによって、液晶層形成用塗布液(1)を調製した。
(1)棒状サーモトロピック液晶化合物(下記化合物(A)):100質量部
(2)キラル剤(下記化合物(B)、Palicolor(登録商標) LC756、BASF社):1.7質量部
(3)光重合開始剤(IRGACURE(登録商標) 907、BASF社):3質量部
(4)光重合開始剤(PM758、日本化薬株式会社):1質量部
(5)配向規制剤(下記化合物(C)):0.5質量部
(6)溶媒(メチルエチルケトン):184質量部
(7)溶媒(シクロヘキサノン):31質量部
配向層を有する基材を70℃で加熱し、次いで、バー(バーの番号:18)を用いて、配向層の上に液晶層形成用塗布液(1)を塗布した。
配向層の上に塗布された液晶層形成用塗布液(1)を、70℃のオーブン内で1分間乾燥することによって塗膜(厚さ:10μm、溶媒の含有率:1質量%以下)を形成した。
塗膜を80℃に加熱した状態で、80℃に加熱したステンレス製ブレードを塗膜に接触させ、次いで、上記塗膜に接触させたまま、上記ブレードを3.0m/分の速度で移動させることによって、上記塗膜に対してせん断力を与えた。上記ブレードの塗膜との接触部の長さは、30mmであった。せん断速度は、2,500秒-1であった。
せん断力を与えた塗膜に対して、メタルハライドランプを用いて紫外線(露光量:500mJ/cm2)を照射することによって、上記塗膜を硬化させた。
以下の手順によって、第1のコレステリック液晶層の上に第2のコレステリック液晶層(厚さ:8μm)を形成した。
下記に示す各成分を混合した後、ポリプロピレン製フィルター(孔径:0.2μm)を用いてろ過することによって、液晶層形成用塗布液(2)を調製した。
(1)棒状サーモトロピック液晶化合物(化合物(A)):100質量部
(2)キラル剤(化合物(B)、Palicolor(登録商標) LC756、BASF社):1.2質量部
(3)光重合開始剤(IRGACURE(登録商標) 907、BASF社):1質量部
(4)光重合開始剤(PM758、日本化薬株式会社):1質量部
(5)配向規制剤(化合物(C)):0.5質量部
(6)溶媒(メチルエチルケトン):184質量部
(7)溶媒(シクロヘキサノン):31質量部
第1のコレステリック液晶層を有する基材を70℃で加熱し、次いで、バー(バーの番手:18)を用いて、第1のコレステリック液晶層の上に液晶層形成用塗布液(2)を塗布した。
第1のコレステリック液晶層の上に塗布された液晶層形成用塗布液(2)を、70℃のオーブン内で1分間乾燥することによって塗膜(厚さ:10μm、溶媒の含有率:1質量%以下)を形成した。
塗膜を70℃に加熱した状態で、70℃に加熱したステンレス製ブレードを塗膜に接触させ、次いで、上記塗膜に接触させたまま、上記ブレードを1.5m/分の速度で移動させることによって、上記塗膜に対してせん断力を与えた。上記ブレードの塗膜との接触部の長さは、30mmであった。せん断速度は、2,500秒-1であった。
せん断力を与えた塗膜に対して、メタルハライドランプを用いて紫外線(露光量:500mJ/cm2)を照射することによって、上記塗膜を硬化させた。
偏光顕微鏡を用いて、実施例1のコレステリック液晶膜の厚さ方向の断面を観察した。各コレステリック液晶層において、暗部及び明部が交互に並んだ縞模様が観察された。第1のコレステリック液晶層と第2のコレステリック液晶層の界面において、上記第2のコレステリック液晶層で観察される暗部は、上記第1のコレステリック液晶層で観察される暗部に接続していた。
液晶層形成用塗布液(1)におけるキラル剤の添加量を1.2質量部に変更したこと以外は、実施例1と同様の手順によって、実施例2のコレステリック液晶膜を製造した。
第2のコレステリック液晶層の形成において、塗膜に対してせん断力を与えずに、乾燥後の塗膜を硬化させたこと以外は、実施例1と同様の手順によって、比較例1のコレステリック液晶膜を製造した。
ヘイズメーター(NDH 2000、日本電色工業株式会社)を用いて、各コレステリック液晶膜のヘイズを測定した。測定結果を表1に示す。
20:第1のコレステリック液晶層
21:第2のコレステリック液晶層
30、31:暗部
40、41:明部
Z:積層方向
Claims (11)
- 顕微鏡を用いて観察される暗部及び明部が交互に並んだ縞模様を有する第1のコレステリック液晶層と、
前記第1のコレステリック液晶層に接して配置され、顕微鏡を用いて観察される暗部及び明部が交互に並んだ縞模様を有する第2のコレステリック液晶層と、を有し、
前記第1のコレステリック液晶層と前記第2のコレステリック液晶層との界面において、前記第2のコレステリック液晶層で観察される前記暗部が、前記第1のコレステリック液晶層で観察される前記暗部に接続している
コレステリック液晶膜。 - 厚さ方向の断面視において、前記第2のコレステリック液晶層で観察される前記暗部のうち隣り合う2つの暗部の距離が、前記第1のコレステリック液晶層で観察される前記暗部のうち隣り合う2つの暗部の距離と異なる請求項1に記載のコレステリック液晶膜。
- 厚さ方向の断面視において、前記第2のコレステリック液晶層で観察される前記暗部のうち隣り合う2つの暗部の距離が、前記第1のコレステリック液晶層で観察される前記暗部のうち隣り合う2つの暗部の距離よりも大きい請求項1又は請求項2に記載のコレステリック液晶膜。
- 厚さ方向の断面視において、前記第1のコレステリック液晶層で観察される前記暗部のうち隣り合う2つの暗部の距離に対する前記第2のコレステリック液晶層で観察される前記暗部のうち隣り合う2つの暗部の距離の比が、1~2である請求項1に記載のコレステリック液晶膜。
- 厚さ方向の断面視において、前記第1のコレステリック液晶層で観察される前記暗部のうち隣り合う2つの暗部の距離が、0.1μm~2μmである請求項1~請求項4のいずれか1項に記載のコレステリック液晶膜。
- 厚さ方向の断面視において、前記第2のコレステリック液晶層で観察される前記暗部のうち隣り合う2つの暗部の距離が、0.1μm~5μmである請求項1~請求項5のいずれか1項に記載のコレステリック液晶膜。
- 前記第1のコレステリック液晶層と前記第2のコレステリック液晶層との界面において、前記第1のコレステリック液晶層で観察される前記暗部に接続している前記第2のコレステリック液晶層で観察される前記暗部の割合が、前記第2のコレステリック液晶層で観察される前記暗部の数に対して、50%~100%である請求項1~請求項6のいずれか1項に記載のコレステリック液晶膜。
- 厚さ方向の断面視において、前記第1のコレステリック液晶層で観察される前記暗部が、前記第1のコレステリック液晶層の主面に対して傾斜しており、かつ、前記第2のコレステリック液晶層で観察される前記暗部が、前記第2のコレステリック液晶層の主面に対して傾斜している請求項1~請求項7のいずれか1項に記載のコレステリック液晶膜。
- 厚さ方向の断面視において、前記第1のコレステリック液晶層で観察される前記暗部の平均角度が、前記第1のコレステリック液晶層の主面に対して、20°~90°である請求項1~請求項8のいずれか1項に記載のコレステリック液晶膜。
- 厚さ方向の断面視において、前記第2のコレステリック液晶層で観察される前記暗部の平均角度が、前記第2のコレステリック液晶層の主面に対して、30°~90°である請求項1~請求項9のいずれか1項に記載のコレステリック液晶膜。
- 前記第1のコレステリック液晶層の前記縞模様が、少なくとも、前記第1のコレステリック液晶層の厚さ方向の断面で観察され、かつ、前記第2のコレステリック液晶層の前記縞模様が、少なくとも、前記第2のコレステリック液晶層の厚さ方向の断面で観察される請求項1~請求項10のいずれか1項に記載のコレステリック液晶膜。
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JP6486116B2 (ja) * | 2014-10-31 | 2019-03-20 | 富士フイルム株式会社 | 光学部材および光学部材を有する画像表示装置 |
JP6481018B2 (ja) * | 2015-02-20 | 2019-03-13 | 富士フイルム株式会社 | 透明スクリーン |
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WO2019182052A1 (ja) * | 2018-03-23 | 2019-09-26 | 富士フイルム株式会社 | コレステリック液晶層の製造方法、コレステリック液晶層、液晶組成物、硬化物、光学異方体、反射層 |
WO2019181247A1 (ja) * | 2018-03-23 | 2019-09-26 | 富士フイルム株式会社 | コレステリック液晶層、積層体、光学異方体、反射膜、コレステリック液晶層の製造方法、偽造防止媒体、および、判定方法 |
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KR20220105168A (ko) | 2022-07-26 |
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